TWI648099B - Method of making colloidal metal nanoparticles - Google Patents

Method of making colloidal metal nanoparticles Download PDF

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TWI648099B
TWI648099B TW106120448A TW106120448A TWI648099B TW I648099 B TWI648099 B TW I648099B TW 106120448 A TW106120448 A TW 106120448A TW 106120448 A TW106120448 A TW 106120448A TW I648099 B TWI648099 B TW I648099B
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solution
reduction reaction
bottomed flask
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aqueous solution
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TW201904658A (en
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盧凌
范貴盛
王振翔
邱群倫
張大為
王證鼎
方俊民
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健鼎科技股份有限公司
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Priority to DE102017116090.6A priority patent/DE102017116090B4/en
Priority to JP2017163380A priority patent/JP6461262B2/en
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/0004—Preparation of sols
    • B01J13/0043—Preparation of sols containing elemental metal
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C18/00—Alloys based on zinc
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C5/00—Alloys based on noble metals
    • C22C5/04—Alloys based on a platinum group metal
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C5/00—Alloys based on noble metals
    • C22C5/06—Alloys based on silver
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
    • B22F1/05—Metallic powder characterised by the size or surface area of the particles
    • B22F1/054—Nanosized particles
    • B22F1/0545—Dispersions or suspensions of nanosized particles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/0466—Alloys based on noble metals
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22C—ALLOYS
    • C22C1/00—Making non-ferrous alloys
    • C22C1/04—Making non-ferrous alloys by powder metallurgy
    • C22C1/0483—Alloys based on the low melting point metals Zn, Pb, Sn, Cd, In or Ga

Abstract

本創作提供一種製備金屬奈米粒子膠體溶液的方法，其包含以下步驟：將一金屬水溶液和一還原劑於一反應容器中混合以形成一混合溶液；加熱該混合溶液以進行還原反應而產生含有複數個金屬奈米粒子、反應殘餘物及氣體的一組合物，其中，該反應殘餘物的體積小於該混合溶液總體積的20％，且同時將該氣體導出該反應容器；再用一介質分散該等金屬奈米粒子以獲得一金屬奈米粒子膠體溶液。藉由將還原反應步驟和分散步驟分開進行，該方法具有簡單、安全、有效率、低成本及高產率等優點。The present invention provides a method for preparing a colloidal solution of a metal nanoparticle, comprising the steps of: mixing an aqueous metal solution and a reducing agent in a reaction vessel to form a mixed solution; heating the mixed solution to carry out a reduction reaction to produce a solution a plurality of metal nanoparticles, a reaction residue and a gas composition, wherein the volume of the reaction residue is less than 20% of the total volume of the mixed solution, and at the same time, the gas is led out of the reaction vessel; The metal nanoparticles are used to obtain a colloidal solution of metal nanoparticles. By separating the reduction reaction step and the dispersion step, the method has the advantages of simplicity, safety, efficiency, low cost, and high productivity.

Description

金屬奈米粒子膠體溶液的製法Method for preparing metal nanoparticle colloidal solution

本創作係有關一種製備金屬奈米粒子膠體溶液的方法。 This creation is directed to a method of preparing a colloidal solution of a metal nanoparticle.

金屬奈米粒子因其小尺寸效應、表面效應及量子尺寸效應而與塊材材料在光學、電磁及化學性質的表現上明顯不同。因此，金屬奈米粒子在材料科學、資訊科學、催化作用以及生命科學領域中被廣泛地應用。近年來，科學家一直積極開發製備金屬奈米粒子的各種方法。製備金屬奈米粒子的方法可以分為三大類：(1)雷射剝蝕法(laser ablation method)，其是採用高能雷射連續照射金屬塊材；(2)金屬蒸氣合成(metal vapor synthesis)，其是使氣態金屬原子在一定條件下凝結而聚集形成；(3)化學還原法(chemical reduction method)，其將溶液中的金屬離子還原成金屬奈米粒子。目前，製備金屬奈米粒子的方法以化學還原法最常用，且該還原反應在水溶液或有機溶劑中進行。 Metal nanoparticles differ significantly from bulk materials in their optical, electromagnetic, and chemical properties due to their small size, surface, and quantum size effects. Therefore, metal nanoparticles are widely used in materials science, information science, catalysis, and life sciences. In recent years, scientists have been actively developing various methods for preparing metal nanoparticles. The methods for preparing metal nanoparticles can be divided into three categories: (1) laser ablation method, which uses a high-energy laser to continuously illuminate a metal block; and (2) a metal vapor synthesis. It is formed by coagulation of gaseous metal atoms under certain conditions; (3) chemical reduction method, which reduces metal ions in the solution to metal nanoparticles. At present, a method of preparing metal nanoparticle is most commonly used by a chemical reduction method, and the reduction reaction is carried out in an aqueous solution or an organic solvent.

由於金屬奈米粒子具有較大的表面積，金屬奈米粒子具有較高的物理和化學活性，容易發生氧化和聚集現象。因此，在製備金屬奈米粒子的化學製劑中，通常會引入各種改性劑或封端劑以控制所製得之金屬奈米粒子的粒徑、形狀、分佈、分散性和穩定性。製備金屬奈米粒子膠體溶液的技術對產品的穩定性和品質有很大的影響。然而，加入這些穩定劑也使得製備方法變得更加複雜。 Due to the large surface area of the metal nanoparticles, the metal nanoparticles have high physical and chemical activity and are prone to oxidation and aggregation. Therefore, in the preparation of metal nanoparticle particles, various modifiers or blocking agents are usually introduced to control the particle size, shape, distribution, dispersibility and stability of the prepared metal nanoparticles. The technique for preparing metal nanoparticle colloidal solutions has a great influence on the stability and quality of the product. However, the addition of these stabilizers also complicates the preparation process.

為了解決上述問題，一些製備方法已被提出。例如美國專利第8048193號記載一種製備金膠體溶液的方法，該方法藉由在一成核步驟之第一金鹽溶液中加入檸檬酸鹽還原劑以形成粒子核膠體溶液，並至少進行一次於包含該粒子核的膠體溶液中加入第二金鹽溶液及抗壞血酸鹽還原劑之生長步驟。雖然前述方法可以製備具有目標粒徑和均勻球形的金膠體溶液，然而前述方法必須使用特定的試劑和限制的步驟；並且若為了得到較大粒徑的金膠體溶液，則必須增加製備方法中的生長步驟次數。因此，前述製備方法仍不夠方便及有效率。 In order to solve the above problems, some preparation methods have been proposed. For example, US Patent No. 8048193 describes a method for preparing a gold colloid solution by adding a citrate reducing agent to a first gold salt solution in a nucleation step to form a particle core colloidal solution, and at least once. A growth step of adding a second gold salt solution and an ascorbate reducing agent to the colloidal solution of the particle core. Although the foregoing method can prepare a gold colloid solution having a target particle diameter and a uniform spherical shape, the foregoing method must use a specific reagent and a limiting step; and if a gold colloidal solution having a larger particle diameter is obtained, it is necessary to increase the preparation method. The number of growth steps. Therefore, the aforementioned preparation method is still insufficiently convenient and efficient.

另外，如美國專利公開案第20120046482號記載一種合成金奈米粒子的方法，該方法藉由將含有金離子的溶液和包含至少兩個羧基的羧酸混合以形成混合物，並在約20℃至60℃的反應溫度下反應。雖然所述方法可以簡單地製備金奈米粒子膠體溶液，但必須使用特定的試劑否則無法達到期望的效果；並且因所述方法限制在相對低的溫度下進行反應，因此需更多時間來完成反應。因此，前述製備方法依舊不夠方便及有效率。 In addition, a method of synthesizing gold nanoparticles by mixing a solution containing gold ions and a carboxylic acid containing at least two carboxyl groups to form a mixture at about 20 ° C is described, for example, in US Patent Publication No. 20120046482. The reaction was carried out at a reaction temperature of 60 °C. Although the method can simply prepare a colloidal solution of gold nanoparticles, it is necessary to use a specific reagent, otherwise the desired effect cannot be achieved; and because the method restricts the reaction at a relatively low temperature, it takes more time to complete reaction. Therefore, the aforementioned preparation method is still not convenient and efficient.

有鑑於習用的製備方法無法方便且有效率地製備金屬奈米粒子膠體溶液，本創作之目的在於提供一種可以簡化製備金屬奈米粒子膠體溶液的方法及系統，其不僅簡單、安全，還能提高時效和成本效益，且其對環境友善，並能提高產率。 In view of the conventional preparation method, the metal nanoparticle colloidal solution cannot be conveniently and efficiently prepared. The purpose of the present invention is to provide a method and system for simplifying the preparation of a metal nanoparticle colloidal solution, which is not only simple, safe, but also improved. Time-sensitive and cost-effective, and it is environmentally friendly and can increase productivity.

為達成前述目的，本創作提供一種製備金屬奈米粒子膠體溶液的方法，其包含步驟(a)至步驟(c)；步驟(a)：將一金屬水溶液和一還原劑於一反應容器中混合以形成一混合溶液；步驟(b)：加熱該混合溶液以進行還原反應，而產生含有複數個金屬奈米粒子、反應殘餘物及氣體的一組合物，其中，該反應殘餘物的體積小於該混合溶液總體積的20%，且將該氣體導出該反應容器； 步驟(c)：再用一介質分散該等金屬奈米粒子，以獲得一金屬奈米粒子膠體溶液。 In order to achieve the foregoing object, the present invention provides a method for preparing a colloidal solution of a metal nanoparticle, comprising the steps (a) to (c); and the step (a): mixing an aqueous metal solution and a reducing agent in a reaction vessel To form a mixed solution; and step (b): heating the mixed solution to carry out a reduction reaction to produce a composition comprising a plurality of metal nanoparticles, a reaction residue, and a gas, wherein the reaction residue has a volume smaller than the Mixing 20% of the total volume of the solution and deriving the gas out of the reaction vessel; Step (c): dispersing the metal nanoparticles with a medium to obtain a metal nanoparticle colloidal solution.

藉由加熱該混合溶液並將從還原反應產生的該氣體導出該反應容器，能促成完全的還原反應，進而提高產率。再者，藉由限制該混合溶液在該反應容器中的體積以增加反應物原子的碰撞概率，而可以加速反應速率。此外，在該等金屬奈米粒子形成的過程中，水溶液中的水會蒸發使得還原步驟與分散步驟無法同時進行。因此，還原劑和分散劑能具有廣泛的選擇而不受限制，使本創作之製備方法能有效簡化金屬奈米粒子膠體溶液的生產。 By heating the mixed solution and deriving the gas generated from the reduction reaction out of the reaction vessel, a complete reduction reaction can be promoted, thereby increasing the yield. Furthermore, the reaction rate can be accelerated by limiting the volume of the mixed solution in the reaction vessel to increase the collision probability of the reactant atoms. Further, during the formation of the metal nanoparticles, the water in the aqueous solution evaporates so that the reduction step and the dispersion step cannot be simultaneously performed. Therefore, the reducing agent and the dispersing agent can have a wide range of choices without limitation, so that the preparation method of the present invention can effectively simplify the production of the colloidal solution of the metal nanoparticle.

根據本創作，該金屬水溶液含有金屬離子，該金屬離子包括金離子、銀離子、銅離子、鋅離子、鎳離子、鈀離子、鈷離子、鐵離子、鈦離子、鎘離子、鉑離子、鋁離子、鉛離子、錳離子、鉻離子、鉬離子、釩離子或鎢離子。 According to the present invention, the aqueous metal solution contains metal ions including gold ions, silver ions, copper ions, zinc ions, nickel ions, palladium ions, cobalt ions, iron ions, titanium ions, cadmium ions, platinum ions, aluminum ions. , lead ions, manganese ions, chromium ions, molybdenum ions, vanadium ions or tungsten ions.

根據本創作，該金屬水溶液還含有陰離子，該陰離子包括鹵離子、氫氧根離子、乙酸根離子、硝酸根離子、硫酸根離子或磷酸根離子。 According to the present invention, the aqueous metal solution further contains an anion including a halide ion, a hydroxide ion, an acetate ion, a nitrate ion, a sulfate ion or a phosphate ion.

舉例而言，該金屬離子來自於四氯金酸(HAuCl4)、硝酸銀(AgNO3)、硝酸銅(Cu(NO3)2)、二氯化銅(CuCl2)、二氯化鋅(ZnCl2)、二氯化鎳(NiCl2)、氯化鈀(PdCl2)、二氯化鈷(CoCl2)、二氯化鐵(FeCl2，又稱氯化亞鐵)、三氯化鐵(FeCl3)、二氯化鈦(TiCl2)或四氯化鈦(TiCl4)。 For example, the metal ion is derived from tetrachloroauric acid (HAuCl 4 ), silver nitrate (AgNO 3 ), copper nitrate (Cu(NO 3 ) 2 ), copper dichloride (CuCl 2 ), zinc dichloride (ZnCl). 2 ), nickel dichloride (NiCl 2 ), palladium chloride (PdCl 2 ), cobalt dichloride (CoCl 2 ), iron dichloride (FeCl 2 , also known as ferrous chloride), ferric chloride ( FeCl 3 ), titanium dichloride (TiCl 2 ) or titanium tetrachloride (TiCl 4 ).

此外，將從還原反應生成的氣體以水捕捉(trap)，因而可收集大量的酸水溶液以便回收再利用而減少酸性廢棄物。 Further, the gas generated from the reduction reaction is trapped with water, so that a large amount of aqueous acid solution can be collected for recycling and reuse to reduce acidic waste.

在一些具體實施例中，使用四氯金酸製造金奈米粒子，並從該還原反應產生的氯化氫氣體以水捕捉以生成回收的鹽酸。 In some embodiments, the gold nanoparticles are produced using tetrachloroauric acid and the hydrogen chloride gas produced from the reduction is captured with water to form recovered hydrochloric acid.

在一些具體實施例中，使用硝酸銀製造銀奈米粒子，並從該還原反應產生的二氧化氮氣體以水捕捉以生成回收的硝酸。 In some embodiments, silver nanoparticles are produced using silver nitrate and the nitrogen dioxide gas produced from the reduction is captured with water to form recovered nitric acid.

反應溫度會影響製備金屬奈米粒子的反應速率。若沒有適當的溫度控制，則前述反應可能會不均勻進行而可能產生氣泡進而影響金屬奈米粒子的品質。 The reaction temperature affects the rate of reaction for preparing the metal nanoparticles. Without proper temperature control, the aforementioned reaction may be uneven and may cause bubbles to affect the quality of the metal nanoparticles.

根據本創作，該步驟(b)中的加熱溫度為50℃至150℃。優選地，該步驟(b)中的加熱溫度為70℃至130℃。 According to the present creation, the heating temperature in the step (b) is from 50 ° C to 150 ° C. Preferably, the heating temperature in the step (b) is from 70 ° C to 130 ° C.

根據本創作，該步驟(c)中的分散溫度為20℃至100℃。優選地，該步驟(c)中的分散溫度為50℃至80℃。 According to the present creation, the dispersion temperature in the step (c) is from 20 ° C to 100 ° C. Preferably, the dispersion temperature in the step (c) is from 50 ° C to 80 ° C.

依據本創作，所述還原劑可包含至少一種酯類。 According to the present creation, the reducing agent may comprise at least one ester.

具體而言，所述酯類選自於一羧酸酯、一環酯、一聚酯及其組合。 Specifically, the ester is selected from the group consisting of monocarboxylates, monocyclic esters, monoesters, and combinations thereof.

優選地，所述羧酸酯為通式(I)所表示的， 其中，通式(I)中的R為氫或甲基，而x為1至16的整數。 Preferably, the carboxylic acid ester is represented by the formula (I) Wherein R in the formula (I) is hydrogen or a methyl group, and x is an integer of from 1 to 16.

優選地，所述環酯為通式(II)所表示的，其中， 通式(II)中的環包含一氧原子及4至6個碳原子，而G為氫、甲基或乙基。 Preferably, the cyclic ester is represented by the formula (II) Wherein the ring of the formula (II) contains an oxygen atom and 4 to 6 carbon atoms, and G is hydrogen, methyl or ethyl.

優選地，所述聚酯為通式(III)所表示的，其 中，通式(III)中的R為氫或甲基，而n為2至1400的整數。 Preferably, the polyester is represented by the formula (III) Wherein R in the formula (III) is hydrogen or a methyl group, and n is an integer of from 2 to 1400.

優選地，所述酯類的組合為一乳酸甲酯(methyl lactate)和一乳酸乙酯(ethyl lactate)、一乳酸甲酯和一γ-丁內酯(γ-butyrolactone)、或一乳酸乙酯和一γ-丁內酯。 Preferably, the combination of the esters is methyl lactate and ethyl lactate, methyl lactate and gamma-butyrolactone, or ethyl lactate. And a γ-butyrolactone.

依據本創作，該還原劑可以包含一檸檬酸(citric acid)、一乳酸(lactic acid)、一乙醇酸(glycolic acid)、一抗壞血酸(ascorbic acid)、一草酸(oxalic acid)、一酒石酸(tartaric acid)、一1,4-丁二醇(1,4-butanediol)、一甘油(glycerol)、一聚乙二醇(poly(ethylene glycol))、一氫醌(hydroquinone)、一乙醛(acetaldehyde)、一葡萄糖(glucose)、一纖維素(cellulose)、一羧甲基纖維素(carboxymethyl cellulose)、一環糊精(cyclodextrin)、一殼多醣(chitin)、一殼聚醣(chitosan)或其組合。 According to the present invention, the reducing agent may comprise a citric acid, a lactic acid, a glycolic acid, an ascorbic acid, or an oxalic acid. Acid), tartaric acid, 1,4-butanediol, glycerol, poly(ethylene glycol), hydroquinone ), acetaldehyde, glucose, cellulose, carboxymethyl cellulose, cyclodextrin, chitin, chitin Chitosan or a combination thereof.

舉例而言，所述還原劑可以包含至少一酯類和至少一非酯類還原劑的組合。 For example, the reducing agent can comprise a combination of at least one ester and at least one non-ester reducing agent.

優選地，所述至少一酯類和所述至少一非酯類還原劑的組合為一乳酸甲酯搭配一乳酸、一檸檬酸、一1,4-丁二醇或一聚乙二醇的組合。 Preferably, the combination of the at least one ester and the at least one non-ester reducing agent is a combination of a methyl lactate and a lactic acid, a citric acid, a 1,4-butanediol or a polyethylene glycol. .

優選地，所述至少一酯類和所述至少一非酯類還原劑的組合為一乳酸乙酯搭配一乳酸、一檸檬酸、一1,4-丁二醇或一聚乙二醇的組合。 Preferably, the combination of the at least one ester and the at least one non-ester reducing agent is a combination of a lactate with a lactic acid, a citric acid, a 1,4-butanediol or a polyethylene glycol. .

優選地，所述至少一酯類和所述至少一非酯類還原劑的組合為一γ-丁內酯搭配一乳酸的組合。 Preferably, the combination of the at least one ester and the at least one non-ester reducing agent is a combination of a γ-butyrolactone and a lactic acid.

具體而言，所述金屬水溶液的體積莫耳濃度為0.1M至3.0M。優選地，所述金屬水溶液的體積莫耳濃度為0.1M至1.0M。更優選地，所述金屬水溶液的體積莫耳濃度為0.2M。 Specifically, the metal aqueous solution has a molar concentration of 0.1 M to 3.0 M. Preferably, the aqueous metal solution has a molar concentration of from 0.1 M to 1.0 M. More preferably, the aqueous metal solution has a molar concentration of 0.2 M.

優選地，該還原劑包含一第一試劑或一聚酯。具體而言，當該還原劑包含該第一試劑時，該第一試劑係選自於一羧酸酯、一環狀酯、一檸檬酸、一乳酸、一乙醇酸、一抗壞血酸、一草酸、一酒石酸、一1,4-丁二醇、一甘油、一氫醌、一乙醛、一葡萄糖、一甲殼質(即殼多醣)及其組合，所述第一試劑相對於該金屬離子的摩耳比為1至40。優選地，所述第一試劑相對於該金屬離子的摩耳比為1至8。更優選地，所述第一試劑相對於該金屬離子的摩耳比為4。 Preferably, the reducing agent comprises a first reagent or a polyester. Specifically, when the reducing agent comprises the first reagent, the first reagent is selected from the group consisting of a monocarboxylic acid ester, a cyclic ester, a citric acid, a monolactic acid, a monoglycolic acid, an ascorbic acid, an oxalic acid, a tartaric acid, a 1,4-butanediol, a monoglycerol, a monohydroquinone, an acetaldehyde, a glucose, a chitin (ie, chitin), and combinations thereof, the first reagent relative to the metal ion The ear ratio is 1 to 40. Preferably, the first reagent has an Alpha ratio of 1 to 8 with respect to the metal ion. More preferably, the molar ratio of the first reagent to the metal ion is four.

具體而言，該還原劑為聚酯時，所述聚酯的重量範圍為30mg至150mg。 Specifically, when the reducing agent is a polyester, the weight of the polyester ranges from 30 mg to 150 mg.

依據本創作，反應時間長短取決於該還原劑的選用種類及反應物的莫耳濃度，該反應的反應時間可為5分鐘至80分鐘。優選地，該反應的反應時間為7分鐘至15分鐘。 According to the present creation, the reaction time depends on the type of the reducing agent selected and the molar concentration of the reactant, and the reaction time of the reaction may be from 5 minutes to 80 minutes. Preferably, the reaction time of the reaction is from 7 minutes to 15 minutes.

舉例而言，金離子的還原反應速率可通過該還原劑的組合來調節，藉以獲得不同大小的複數個金奈米粒子。 For example, the rate of reduction of gold ions can be adjusted by a combination of the reducing agents to obtain a plurality of gold nanoparticles of different sizes.

依據本創作，該步驟(c)中用以分散該等金屬奈米粒子的介質可以是水或含有分散劑的水溶液。具體而言，所述分散劑水溶液可以是一檸檬酸水溶液、一乳酸水溶液、一聚乳酸水溶液(aqueous poly(lactic acid))、一氫氧化鈉水溶液(aqueous sodium hydroxide、一十六烷基胺水溶液(aqueous hexadecylamine)、一油胺水溶液(aqueous oleylamine)、一四辛基溴化銨水溶液(aqueous tetraoctylammonium bromide,TOAB)、一十二烷硫醇水溶液(aqueous dodecanethiol)、一聚環氧乙烷水溶液(aqueous poly(ethylene oxide))、一聚乙烯吡咯烷酮水溶液(aqueous polyvinylpyrrolidone,PVP)或其組合。 According to the present invention, the medium for dispersing the metal nanoparticles in the step (c) may be water or an aqueous solution containing a dispersing agent. Specifically, the aqueous solution of the dispersing agent may be an aqueous solution of citric acid, an aqueous solution of lactic acid, an aqueous poly(lactic acid), an aqueous solution of aqueous sodium hydroxide or an aqueous solution of hexadecylamine. (aqueous hexadecylamine), aqueous oleylamine, aqueous tetraoctylammonium bromide (TOAB), aqueous dodecanethiol, aqueous solution of polyethylene oxide ( Aqueous poly(ethylene oxide)), an aqueous polyvinylpyrrolidone (PVP) or a combination thereof.

所述分散劑的體積莫耳濃度為0.001M至0.1M。優選地，所述分散劑的體積莫耳濃度為0.01M至0.05M。 The dispersant has a molar concentration of from 0.001 M to 0.1 M. Preferably, the dispersant has a molar concentration of from 0.01 M to 0.05 M.

舉例而言，所述分散劑與所述金屬奈米粒子的莫耳比為10至100。優選地，所述分散劑與所述金屬奈米粒子的莫耳比為15至30。 For example, the molar ratio of the dispersant to the metal nanoparticles is from 10 to 100. Preferably, the molar ratio of the dispersant to the metal nanoparticles is from 15 to 30.

依據本創作，所有水溶液所使用的水均為蒸餾水。優選地，所述的水為去離子水。 According to the present creation, the water used in all aqueous solutions is distilled water. Preferably, the water is deionized water.

在進行步驟(b)中的還原反應以及在該步驟(c)中的分散步驟時，其水中僅使用有機還原劑和有機分散劑而不使用無機陽離子(例如Na+或K+)是有 益的，因為所獲得之金屬奈米粒子膠體溶液將可免除無機陽離子的干擾而獲得良好的穩定性。 It is advantageous to carry out the reduction reaction in the step (b) and the dispersion step in the step (c), using only an organic reducing agent and an organic dispersing agent in the water without using an inorganic cation such as Na + or K + . Because the obtained metal nanoparticle colloidal solution will be able to avoid the interference of inorganic cations and obtain good stability.

依據本創作，所述還原反應進行時，會以實地紅外線光譜分析(infrared(IR)spectral analysis on-site)即時監測。在IR光譜中，約1500cm-1至500cm-1的區域包含非常複雜的一系列吸收峰，其主要是由於所有的分子內鍵振動方式的結果，而該區域稱為指紋辨識區。該指紋辨識區的重要性在於，每個不同的物質在所述指紋辨識區的光譜會產生不同的波谷圖案。因此，當波谷圖案與一開始的所述混合溶液不同時意味著反應仍在進行，而當所述波谷圖案不再有明顯變化時，表示該混合溶液中的反應已完成。 According to the present creation, when the reduction reaction is carried out, it is immediately monitored by infrared (IR) spectral analysis on-site. In the IR spectrum, a region of about 1500 cm -1 to 500 cm -1 contains a very complex series of absorption peaks, mainly due to the result of all intramolecular bond vibration modes, which are called fingerprint recognition regions. The importance of the fingerprint identification area is that each different substance produces a different trough pattern in the spectrum of the fingerprint recognition area. Therefore, when the trough pattern is different from the initial mixed solution, it means that the reaction is still going on, and when the trough pattern is no longer significantly changed, it means that the reaction in the mixed solution is completed.

依據本創作，該金屬奈米粒子膠體溶液中的粒子尺寸可通過紫外光-可見光(UV-Vis)光譜的吸收峰來做為特徵，因為在UV-Vis光譜中，各金屬奈米粒子膠體溶液的吸收最大值之波長(λmax)具有其特定的範圍。 According to the present invention, the particle size in the colloidal solution of the metal nanoparticle can be characterized by the absorption peak of the ultraviolet-visible (UV-Vis) spectrum, because in the UV-Vis spectrum, each metal nanoparticle colloidal solution The wavelength of the absorption maximum (λ max ) has its specific range.

具體而言，該金奈米粒子膠體溶液的λmax為515nm至572nm。 Specifically, the λ max of the gold nanoparticle colloidal solution is 515 nm to 572 nm.

具體而言，該銀奈米粒子膠體溶液的λmax為370nm至420nm。 Specifically, the silver nanoparticle colloidal solution has a λ max of 370 nm to 420 nm.

依據本創作，該金屬奈米粒子膠體溶液中的粒子尺寸也會影響UV-Vis光譜中的λmax。當所述奈米粒子的尺寸增加時，其λmax的波長也會變大。例如，對應λmax為525nm的金奈米粒子膠體溶液，其平均尺寸為26nm±1nm，而對應λmax為530nm的金奈米粒子膠體溶液，其平均尺寸為30nm±1nm。 According to the present creation, the particle size in the colloidal solution of the metal nanoparticle also affects λ max in the UV-Vis spectrum. As the size of the nanoparticle increases, the wavelength of λ max also becomes larger. For example, a colloidal solution of a gold nanoparticle having a λ max of 525 nm has an average size of 26 nm ± 1 nm, and a colloidal solution of a gold nanoparticle corresponding to a λ max of 530 nm has an average size of 30 nm ± 1 nm.

依據本創作，該金屬奈米粒子的粒子尺寸也可透過穿透式電子顯微鏡(transmission electron microscopy,TEM)的影像做為特徵。 According to the present creation, the particle size of the metal nanoparticle can also be characterized by an image of a transmission electron microscopy (TEM).

依據本創作，所述金屬奈米粒子膠體溶液顯示高界達電位(zeta potential)，而界達電位是膠體溶液穩定性的重要指標。 According to the present invention, the metal nanoparticle colloidal solution exhibits a high zeta potential, and the boundary potential is an important indicator of the stability of the colloidal solution.

從以下內容並結合附圖的詳細說明，使得本創作的其他目的、優點及新穎特徵變得更加明顯。 Other objects, advantages and novel features of the present invention will become apparent from the Detailed Description of the Drawing.

圖1為本創作之製備金屬奈米粒子膠體溶液的方法之流程示意圖。 FIG. 1 is a schematic flow chart of a method for preparing a colloidal solution of a metal nanoparticle according to the present invention.

圖2為本創作實施例2中所得之金奈米粒子膠體溶液的UV-Vis光譜。 2 is a UV-Vis spectrum of the colloidal solution of the gold nanoparticles obtained in the creation of Example 2.

圖3A為實施例2中所得之金奈米粒子膠體溶液的FT-IR光譜(如細線所示)及在130℃下加熱乳酸甲酯與HCl水溶液12分鐘之產物的FT-IR光譜(如粗線所示)。 3A is an FT-IR spectrum (shown by a thin line) of a colloidal solution of a gold nanoparticle obtained in Example 2, and an FT-IR spectrum of a product obtained by heating a methyl lactate and an aqueous HCl solution at 130 ° C for 12 minutes (eg, coarse) Line shown).

圖3B為在130℃下加熱乳酸甲酯與HCl水溶液12分鐘之產物的FT-IR光譜(如細線所示)及在起始物之乳酸甲酯的FT-IR光譜(如粗線所示)。 Figure 3B is an FT-IR spectrum (shown by thin lines) of the product of heating methyl lactate and aqueous HCl for 12 minutes at 130 ° C and the FT-IR spectrum of the methyl lactate in the starting material (as indicated by the thick line) .

圖4為本創作實施例5中所得之金奈米粒子膠體溶液的UV-Vis光譜。 4 is a UV-Vis spectrum of the colloidal solution of the gold nanoparticles obtained in the creation of Example 5.

圖5為本創作實施例5中所得之金奈米粒子的TEM影像圖(平均粒徑為22nm至23nm)。 Fig. 5 is a TEM image of the gold nanoparticles obtained in the fifth embodiment (average particle diameter: 22 nm to 23 nm).

圖6為本創作實施例15中所得之金奈米粒子膠體溶液的UV-Vis光譜。 Fig. 6 is a UV-Vis spectrum of the colloidal solution of the gold nanoparticles obtained in Inventive Example 15.

圖7A為實施例15中所得之金奈米粒子膠體溶液的FT-IR光譜(如細線所示)及在130℃下加熱乳酸乙酯與HCl水溶液12分鐘之產物的FT-IR光譜(如粗線所示)。 7A is an FT-IR spectrum (as indicated by a thin line) of a colloidal solution of a gold nanoparticle obtained in Example 15, and an FT-IR spectrum of a product obtained by heating an ethyl lactate and an aqueous HCl solution at 130 ° C for 12 minutes (eg, coarse) Line shown).

圖7B為在130℃下加熱乳酸乙酯與HCl水溶液12分鐘之產物的FT-IR光譜(如細線所示)及在起始物之乳酸乙酯的FT-IR光譜(如粗線所示)。 Figure 7B is an FT-IR spectrum (shown by thin lines) of the product of heating ethyl lactate and HCl in water at 130 ° C for 12 minutes and the FT-IR spectrum of the ethyl lactate in the starting material (as indicated by the thick line) .

圖8為本創作實施例23中所得之金奈米粒子膠體溶液的UV-Vis光譜。 Figure 8 is a UV-Vis spectrum of the colloidal solution of the gold nanoparticles obtained in Inventive Example 23.

圖9為本創作實施例23中所得之金奈米粒子的TEM影像圖(平均粒徑為33nm至34nm)。 Fig. 9 is a TEM image of the gold nanoparticles obtained in Inventive Example 23 (average particle diameter: 33 nm to 34 nm).

圖10為本創作實施例27中所得之金奈米粒子膠體溶液的UV-Vis光譜。 Figure 10 is a UV-Vis spectrum of the colloidal solution of the gold nanoparticles obtained in Inventive Example 27.

圖11A為實施例27中所得之金奈米粒子膠體溶液的FT-IR光譜(如粗線所示)及在130℃下加熱γ-丁內酯與HCl水溶液30分鐘之產物的FT-IR光譜(如細線所示)。 Figure 11A is an FT-IR spectrum of the colloidal solution of the gold nanoparticle obtained in Example 27 (shown as a thick line) and FT-IR spectrum of the product of heating γ -butyrolactone and HCl aqueous solution at 130 ° C for 30 minutes. (as shown by the thin line).

圖11B為在130℃下加熱γ-丁內酯與HCl水溶液30分鐘之產物的FT-IR光譜(如細線所示)及在起始物之γ-丁內酯的FT-IR光譜(如粗線所示)。 Figure 11B is an FT-IR spectrum (shown by thin lines) of the product of heating γ -butyrolactone and HCl aqueous solution at 130 ° C for 30 minutes and FT-IR spectrum of γ -butyrolactone in the starting material (such as coarse Line shown).

圖12為本創作實施例27中所得之金奈米粒子的TEM影像圖(平均粒徑為27nm至28nm)。 Fig. 12 is a TEM image of the gold nanoparticles obtained in Inventive Example 27 (average particle diameter: 27 nm to 28 nm).

圖13為本創作實施例33中所得之金奈米粒子膠體溶液的UV-Vis光譜。 Figure 13 is a UV-Vis spectrum of the colloidal solution of the gold nanoparticles obtained in Inventive Example 33.

圖14A為實施例33中所得之金奈米粒子膠體溶液的FT-IR光譜(如粗線所示)及在130℃下加熱聚乳酸與HCl水溶液30分鐘之產物的FT-IR光譜(如細線所示)。 14A is an FT-IR spectrum (shown by a thick line) of a colloidal solution of a gold nanoparticle obtained in Example 33, and an FT-IR spectrum (such as a fine line) of a product obtained by heating a polylactic acid and an aqueous HCl solution at 130 ° C for 30 minutes. Shown).

圖14B為起始物之聚乳酸的FT-IR光譜。 Figure 14B is an FT-IR spectrum of the polylactic acid of the starting material.

圖15為本創作實施例35中所得之金奈米粒子膠體溶液的UV-Vis光譜。 Figure 15 is a UV-Vis spectrum of the colloidal solution of the gold nanoparticles obtained in Inventive Example 35.

圖16為本創作實施例37中所得之金奈米粒子膠體溶液的UV-Vis光譜。 Figure 16 is a UV-Vis spectrum of the colloidal solution of the gold nanoparticles obtained in Inventive Example 37.

圖17A為實施例37中所得之金奈米粒子膠體溶液的FT-IR光譜(如細線所示)及在130℃下加熱乳酸與HCl水溶液12分鐘之產物的FT-IR光譜(如粗線所示)。 Figure 17A is an FT-IR spectrum of the colloidal solution of the gold nanoparticles obtained in Example 37 (as indicated by the thin line) and an FT-IR spectrum of the product of heating the aqueous solution of lactic acid and HCl for 12 minutes at 130 ° C (such as a thick line) Show).

圖17B為在130℃下加熱乳酸與HCl水溶液12分鐘之產物的FT-IR光譜(如細線所示)及在起始物之乳酸的FT-IR光譜(如粗線所示)。 Figure 17B is an FT-IR spectrum (shown by thin lines) of the product of heating the aqueous solution of lactic acid and HCl for 12 minutes at 130 ° C and the FT-IR spectrum of the lactic acid in the starting material (as indicated by the thick line).

圖18為實施例37中所得之金奈米粒子膠體溶液的界達電位圖。 Figure 18 is a diagram showing the boundary potential of the colloidal solution of the gold nanoparticles obtained in Example 37.

圖19為本創作實施例38中所得之金奈米粒子膠體溶液的UV-Vis光譜。 Figure 19 is a UV-Vis spectrum of the colloidal solution of the gold nanoparticles obtained in Inventive Example 38.

圖20為本創作實施例44中所得之金奈米粒子膠體溶液的UV-Vis光譜。 Figure 20 is a UV-Vis spectrum of the colloidal solution of the gold nanoparticles obtained in Inventive Example 44.

圖21為本創作實施例45中所得之金奈米粒子膠體溶液的UV-Vis光譜。 Figure 21 is a UV-Vis spectrum of the colloidal solution of the gold nanoparticles obtained in Inventive Example 45.

圖22為本創作實施例46中所得之金奈米粒子膠體溶液的UV-Vis光譜。 Figure 22 is a UV-Vis spectrum of the colloidal solution of the gold nanoparticles obtained in Inventive Example 46.

圖23為本創作實施例47中所得之金奈米粒子膠體溶液的UV-Vis光譜。 Figure 23 is a UV-Vis spectrum of the colloidal solution of the gold nanoparticles obtained in Inventive Example 47.

圖24為本創作實施例47中所得之金奈米粒子的TEM影像圖(平均粒徑為38nm至39nm)。 Fig. 24 is a TEM image of the gold nanoparticles obtained in Inventive Example 47 (average particle diameter: 38 nm to 39 nm).

圖25為本創作實施例58中所得之銀奈米粒子膠體溶液的UV-Vis光譜。 Figure 25 is a UV-Vis spectrum of the colloidal solution of silver nanoparticles obtained in Inventive Example 58.

圖26為本創作實施例58中所得之銀奈米粒子的TEM影像圖(平均粒徑為10nm至11nm)。 Figure 26 is a TEM image of the silver nanoparticles obtained in Inventive Example 58 (average particle diameter: 10 nm to 11 nm).

圖27為本創作實施例59中所得之銀奈米粒子膠體溶液的UV-Vis光譜。 Figure 27 is a UV-Vis spectrum of the colloidal solution of silver nanoparticles obtained in Inventive Example 59.

圖28為本創作實施例60中所得之銀奈米粒子膠體溶液的UV-Vis光譜。 Figure 28 is a UV-Vis spectrum of the colloidal solution of silver nanoparticles obtained in Inventive Example 60.

圖29為本創作實施例61中所得之銀奈米粒子膠體溶液的UV-Vis光譜。 Figure 29 is a UV-Vis spectrum of the colloidal solution of silver nanoparticles obtained in Inventive Example 61.

圖30為本創作實施例65中所得之鈀奈米粒子的TEM影像圖(平均粒徑為9nm至10nm)。 Figure 30 is a TEM image of the palladium nanoparticle obtained in Inventive Example 65 (average particle diameter: 9 nm to 10 nm).

圖31為本創作實施例71中所得之鋅奈米粒子的TEM影像圖(平均粒徑為26nm至27nm)。 Figure 31 is a TEM image of the zinc nanoparticles obtained in Inventive Example 71 (average particle diameter: 26 nm to 27 nm).

在下文中，本領域技術人員可從以下實施例很輕易地理解本創作所能達到的優點及效果。因此，應當理解本文提出的敘述僅僅用於說明優選的實施方式而不是用於侷限本創作的範圍，在不悖離本創作的精神和範圍的情況下，可以進行各種修飾、變更以便實施或應用本創作之內容。 Hereinafter, those skilled in the art can easily understand the advantages and effects that can be achieved by the present invention from the following embodiments. Therefore, it is to be understood that the descriptions of the present invention are only intended to illustrate the preferred embodiments and are not intended to limit the scope of the present invention. The content of this creation.

製備金屬奈米粒子膠體溶液的方法 Method for preparing metal nanoparticle colloidal solution

在以下實施例中，使用型號為Agilent Technologies Cary630的傅立葉變換紅外線光譜儀(Fourier transform(FT)-IR spectrometer)記錄紅外線光譜。使用型號為Agilent Technologies Cary60的紫外線-可見光分光光度計(UV-Vis spectrophotometer)量測紫外線-可見光光譜。使用型號為Hitachi H-7100的穿透式顯微鏡(Transmission electron microscopy,TEM)記錄影像。所有使用的試劑皆為試劑級，不需進一步純化即可使用。四氯金酸(HAuCl4,0.2M水溶液)和鋅 粉購自Acros Organics，硝酸銀(AgNO3,0.1M水溶液)購自Merck & Co.，氯化鈀(PdCl2，包含鈀59.4%)購自Uni Region Bio-Tech。超純水購自Hao Feng Biotech Co.。 In the following examples, infrared spectra were recorded using a Fourier transform infrared spectrometer (Fourier transform (FT)-IR spectrometer) model Agilent Technologies Cary 630. The UV-visible spectrum was measured using a UV-Vis spectrophotometer model Agilent Technologies Cary60. Images were recorded using a transmission electron microscopy (TEM) model number Hitachi H-7100. All reagents used were reagent grade and could be used without further purification. Tetrachloroauric acid (HAuCl 4 , 0.2 M aqueous solution) and zinc powder were purchased from Acros Organics, silver nitrate (AgNO 3 , 0.1 M aqueous solution) was purchased from Merck & Co., and palladium chloride (PdCl 2 , containing palladium 59.4%) was purchased from Uni Region Bio-Tech. Ultrapure water was purchased from Hao Feng Biotech Co.

實施例1 使用乳酸甲酯作為還原劑和分散劑以合成金奈米粒子膠體溶液 Example 1 Using methyl lactate as a reducing agent and dispersing agent to synthesize a colloidal solution of gold nanoparticles

以下，使用圖1所示的製備方法進行金奈米粒子膠體溶液的製備程序。 Hereinafter, a preparation procedure of the gold nanoparticle colloidal solution was carried out using the production method shown in FIG.

首先，在步驟(a)中，從入料口將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和乳酸甲酯(22.3毫克，0.21毫莫耳)加入100毫升的雙頸平底燒瓶中，並混合成一混合溶液。 First, in step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and methyl lactate (22.3 mg, 0.21 mmol) were added to a 100 ml two-necked flat-bottomed flask from the feed port. And mixed into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱30分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 30 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有乳酸甲酯(200毫克，1.9毫莫耳)的水溶液50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，其顯示UV-Vis光譜中的λmax為550nm且其O.D.值為0.365。 Finally, in step (c), the aforementioned gold nanoparticles are dispersed in the double-necked flat-bottomed flask using 50 ml of an aqueous solution containing methyl lactate (200 mg, 1.9 mmol) as a medium, and The solution was heated at 70 ° C for 10 minutes to obtain a gold nanoparticle colloidal solution which showed λ max in the UV-Vis spectrum of 550 nm and an OD value of 0.365.

實施例2 使用乳酸甲酯作為還原劑和檸檬酸做為分散劑以合成金奈米粒子膠體溶液 Example 2 Using methyl lactate as a reducing agent and citric acid as a dispersing agent to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和乳酸甲酯(20.6毫克，0.20毫莫耳)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and methyl lactate (20.6 mg, 0.20 mmol) were added to a 100 ml two-necked flat-bottomed flask and mixed into a mixed solution. .

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱15分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 15 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(200毫克，1.0毫莫耳)的水溶液50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，如圖2所示，其在UV-Vis光譜中的λmax為545nm且其以稀釋50%的稀釋液量測反推得知O.D.值為3.896。此外，以FT-IR光譜證實金奈米粒子膠體溶液的形成如圖3A所示。 Finally, in step (c), the aforementioned gold nanoparticles were dispersed in the double-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (200 mg, 1.0 mmol) as a medium, and the solution was Heating at 70 ° C for 10 minutes, a gold nanoparticle colloidal solution was obtained, as shown in Figure 2, its λ max in the UV-Vis spectrum was 545 nm and it was inversely deduced to obtain OD by dilution of 50% dilution. The value is 3.896. Further, the formation of the colloidal solution of the gold nanoparticles by FT-IR spectroscopy was confirmed as shown in Fig. 3A.

實施例3 使用乳酸甲酯作為還原劑和檸檬酸做為分散劑而不加熱分散以合成金奈米粒子膠體溶液 Example 3 Using methyl lactate as a reducing agent and citric acid as a dispersing agent without heating to disperse to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和乳酸甲酯(20.8毫克，0.20毫莫耳)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and methyl lactate (20.8 mg, 0.20 mmol) were added to a 100 ml two-necked flat-bottomed flask and mixed into a mixed solution. .

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱12分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 12 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(200毫克，1.0毫莫耳)的水溶液50毫升作為介質，將前述的金奈米粒子在室溫下分散於該雙頸平底燒瓶中10分鐘，得到一金奈米粒子膠體溶液，其UV-Vis光譜中的λmax為545nm且其所測得的O.D.值為1.784。 Finally, in step (c), 50 ml of an aqueous solution containing citric acid (200 mg, 1.0 mmol) was used as a medium, and the aforementioned gold nanoparticles were dispersed in the double-necked flat-bottomed flask at room temperature for 10 minutes. A gold nanoparticle colloidal solution having a λ max in the UV-Vis spectrum of 545 nm and an OD value of 1.784 was obtained.

實施例4 使用乳酸甲酯和1,4-丁二醇作為組合還原劑以合成金奈米粒子膠體溶液 Example 4 Using methyl lactate and 1,4-butanediol as a combined reducing agent to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和乳酸甲酯(10.7毫克，0.10毫莫耳)及1,4-丁二醇(10.2毫克，0.11毫莫耳)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and methyl lactate (10.7 mg, 0.10 mmol) and 1,4-butanediol (10.2 mg, 0.11) Millions of a two-neck flat-bottomed flask were added and mixed into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱10.5分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 10.5 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(200毫克，1.0毫莫耳)的水溶液50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，其UV-Vis光譜中的λmax為530nm且其所測得的O.D.值為1.258。 Finally, in step (c), the aforementioned gold nanoparticles were dispersed in the double-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (200 mg, 1.0 mmol) as a medium, and the solution was Heating at 70 ° C for 10 minutes gave a colloidal solution of gold nanoparticles having a λ max of 530 nm in the UV-Vis spectrum and an OD value of 1.258.

實施例5 使用乳酸甲酯和檸檬酸作為組合還原劑以合成金奈米粒子膠體溶液 Example 5 Using methyl lactate and citric acid as a combined reducing agent to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和乳酸甲酯(14.7毫克，0.14毫莫耳)及檸檬酸(20.9毫克，0.11毫莫耳)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and methyl lactate (14.7 mg, 0.14 mmol) and citric acid (20.9 mg, 0.11 mmol) were added. A 100 ml two-necked flat-bottomed flask was mixed and mixed into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱10.5分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 10.5 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(200毫克，1.0毫莫耳)的水溶液50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，如圖4所示，其在UV-Vis光譜中的λmax為525nm且其以稀釋50%的稀釋液量測反推得知O.D.值為2.274。此外，如圖5的TEM影像所示，該金奈米粒子之平均粒徑為22nm至23nm。 Finally, in step (c), the aforementioned gold nanoparticles were dispersed in the double-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (200 mg, 1.0 mmol) as a medium, and the solution was Heating at 70 ° C for 10 minutes, a gold nanoparticle colloidal solution was obtained, as shown in Figure 4, its λ max in the UV-Vis spectrum was 525 nm and it was inversely deduced to obtain OD by dilution of 50% dilution. The value is 2.274. Further, as shown in the TEM image of FIG. 5, the average particle diameter of the gold nanoparticles is 22 nm to 23 nm.

實施例6 使用乳酸甲酯和PEG800作為組合還原劑以合成金奈米粒子膠體溶液 Example 6 Using methyl lactate and PEG800 as a combined reducing agent to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和乳酸甲酯(12.1毫克，0.12毫莫耳)及PEG800(80.4毫克)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and methyl lactate (12.1 mg, 0.12 mmol) and PEG 800 (80.4 mg) were added to a 100 ml double neck flat bottom. The flasks were mixed and mixed into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱15.5分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 15.5 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(200毫克，1.0毫莫耳)的水溶液50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，其UV-Vis光譜中的λmax為525nm且其所測得的O.D.值為3.172。 Finally, in step (c), the aforementioned gold nanoparticles were dispersed in the double-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (200 mg, 1.0 mmol) as a medium, and the solution was Heating at 70 ° C for 10 minutes gave a colloidal solution of gold nanoparticles having a λ max of 525 nm in the UV-Vis spectrum and an OD value of 3.172 measured.

實施例7 使用乳酸甲酯和PEG1000作為組合還原劑以合成金奈米粒子膠體溶液 Example 7 Using methyl lactate and PEG1000 as a combined reducing agent to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和乳酸甲酯(11.2毫克，0.12毫莫耳)及PEG1000(106.3毫克)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and methyl lactate (11.2 mg, 0.12 mmol) and PEG 1000 (106.3 mg) were added to a 100 ml double neck flat bottom. The flasks were mixed and mixed into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱15.5分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 15.5 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(200毫克，1.0毫莫耳)的水溶液50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，其UV-Vis光譜中的λmax為525nm且其所測得的O.D.值為3.118。 Finally, in step (c), the aforementioned gold nanoparticles were dispersed in the double-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (200 mg, 1.0 mmol) as a medium, and the solution was Heating at 70 ° C for 10 minutes gave a colloidal solution of gold nanoparticles having a λ max of 525 nm in the UV-Vis spectrum and an OD value of 3.118.

實施例8 使用乳酸甲酯和PEG4000作為組合還原劑以合成金奈米粒子膠體溶液 Example 8 Using methyl lactate and PEG4000 as a combined reducing agent to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和乳酸甲酯(12.1毫克，0.12毫莫耳)及PEG4000(402.7毫克)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and methyl lactate (12.1 mg, 0.12 mmol) and PEG 4000 (402.7 mg) were added to a 100 ml double neck flat bottom. The flasks were mixed and mixed into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱30分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 30 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(200毫克，1.0毫莫耳)的水溶液50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，其UV-Vis光譜中的λmax為530nm且其所測得的O.D.值為3.412。 Finally, in step (c), the aforementioned gold nanoparticles were dispersed in the double-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (200 mg, 1.0 mmol) as a medium, and the solution was Heating at 70 ° C for 10 minutes gave a colloidal solution of gold nanoparticles having a λ max of 530 nm in the UV-Vis spectrum and an OD value of 3.412.

實施例9 使用乳酸甲酯和PEG8000作為組合還原劑以合成金奈米粒子膠體溶液 Example 9 Using methyl lactate and PEG 8000 as a combined reducing agent to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和乳酸甲酯(11.6毫克，0.11毫莫耳)及PEG8000(808.2毫克)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and methyl lactate (11.6 mg, 0.11 mmol) and PEG 8000 (808.2 mg) were added to a 100 ml double neck flat bottom. The flasks were mixed and mixed into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱30分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 30 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(200毫克，1.0毫莫耳)的水溶液50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，其UV-Vis光譜中的λmax為535nm且其所測得的O.D.值為2.952。 Finally, in step (c), the aforementioned gold nanoparticles were dispersed in the double-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (200 mg, 1.0 mmol) as a medium, and the solution was Heating at 70 ° C for 10 minutes gave a colloidal solution of gold nanoparticles having a λ max of 535 nm in the UV-Vis spectrum and an OD value of 2.952.

實施例10 使用乳酸甲酯和PEG10000作為組合還原劑以合成金奈米粒子膠體溶液 Example 10 Using methyl lactate and PEG 10000 as a combined reducing agent to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和乳酸甲酯(11毫克，0.11毫莫耳)及PEG10000(1.003克)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and methyl lactate (11 mg, 0.11 mmol) and PEG 10000 (1.003 g) were added to a 100 ml double neck flat bottom. The flasks were mixed and mixed into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱30分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 30 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(200毫克，1.0毫莫耳)的水溶液50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，其UV-Vis光譜中的λ max為530nm且其所測得的O.D.值為3.028。 Finally, in step (c), the aforementioned gold nanoparticles were dispersed in the double-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (200 mg, 1.0 mmol) as a medium, and the solution was Heating at 70 ° C for 10 minutes gave a colloidal solution of gold nanoparticles having a λ max of 530 nm in the UV-Vis spectrum and an OD value of 3.028.

實施例11 使用乳酸甲酯和PEG11000作為組合還原劑以合成金奈米粒子膠體溶液 Example 11 Using methyl lactate and PEG 11000 as a combined reducing agent to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和乳酸甲酯(11.9毫克，0.11毫莫耳)及PEG11000(1.104克)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and methyl lactate (11.9 mg, 0.11 mmol) and PEG 11000 (1.104 g) were added to a 100 ml double neck flat bottom. The flasks were mixed and mixed into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱30分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 30 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(200毫克，1.0毫莫耳)的水溶液50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，其UV-Vis光譜中的λ max為535nm且其所測得的O.D.值為3.548。 Finally, in step (c), the aforementioned gold nanoparticles were dispersed in the double-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (200 mg, 1.0 mmol) as a medium, and the solution was Heating at 70 ° C for 10 minutes gave a colloidal solution of gold nanoparticles having a λ max of 535 nm in the UV-Vis spectrum and an OD value of 3.548.

實施例12 使用乳酸甲酯和乳酸作為組合還原劑以合成金奈米粒子膠體溶液 Example 12 Using methyl lactate and lactic acid as a combined reducing agent to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和乳酸甲酯(11.8毫克，0.11毫莫耳)及乳酸(13.1毫克，0.15毫莫耳)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and methyl lactate (11.8 mg, 0.11 mmol) and lactic acid (13.1 mg, 0.15 mmol) were added to 100. A two-neck flat-bottomed flask of cc was mixed and mixed into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱15分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 15 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(200毫克，1.0毫莫耳)的水溶液50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，其UV-Vis光譜中的λmax為530nm且其所測得的O.D.值為3.49。 Finally, in step (c), the aforementioned gold nanoparticles were dispersed in the double-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (200 mg, 1.0 mmol) as a medium, and the solution was Heating at 70 ° C for 10 minutes gave a colloidal solution of gold nanoparticles having a λ max of 530 nm in the UV-Vis spectrum and an OD value of 3.49.

實施例13 使用乳酸甲酯和乳酸乙酯作為組合還原劑以合成金奈米粒子膠體溶液 Example 13 Using methyl lactate and ethyl lactate as a combined reducing agent to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和乳酸甲酯(10.4毫克，0.10毫莫耳)及乳酸乙酯(13.1毫克，0.11毫莫耳)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and methyl lactate (10.4 mg, 0.10 mmol) and ethyl lactate (13.1 mg, 0.11 mmol) A 100 ml two-necked flat-bottomed flask was added and mixed into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱8.5分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 8.5 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(200毫克，1.0毫莫耳)的水溶液50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，其UV-Vis光譜中的λmax為530nm且其所測得的O.D.值為1.844。 Finally, in step (c), the aforementioned gold nanoparticles were dispersed in the double-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (200 mg, 1.0 mmol) as a medium, and the solution was Heating at 70 ° C for 10 minutes gave a colloidal solution of gold nanoparticles having a λ max of 530 nm in the UV-Vis spectrum and an OD value of 1.844.

實施例14 使用乳酸乙酯作為還原劑和分散劑以合成金奈米粒子膠體溶液 Example 14 Using ethyl lactate as a reducing agent and dispersing agent to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和乳酸乙酯(26.7毫克，0.23毫莫耳)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and ethyl lactate (26.7 mg, 0.23 mmol) were added to a 100 ml two-necked flat-bottomed flask and mixed into a mixed solution. .

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱12分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 12 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有乳酸乙酯(200毫克，1.7毫莫耳)的水溶液50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，其UV-Vis光譜中的λmax為555nm且其所測得的O.D.值為0.397。 Finally, in step (c), the aforementioned gold nanoparticles are dispersed in the double-necked flat-bottomed flask using 50 ml of an aqueous solution containing ethyl lactate (200 mg, 1.7 mmol) as a medium, and the The solution was heated at 70 ° C for 10 minutes to obtain a gold nanoparticle colloidal solution having a λ max of 555 nm in the UV-Vis spectrum and an OD value of 0.397.

實施例15 使用乳酸乙酯作為還原劑和檸檬酸做為分散劑以合成金奈米粒子膠體溶液 Example 15 Using ethyl lactate as a reducing agent and citric acid as a dispersing agent to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和乳酸乙酯(25.9毫克，0.22毫莫耳)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and ethyl lactate (25.9 mg, 0.22 mmol) were added to a 100 ml two-necked flat-bottomed flask and mixed into a mixed solution. .

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱10分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 10 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(200毫克，1.0毫莫耳)的水溶液50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，如圖6所示，其在UV-Vis光譜中的λmax為525nm且其所測得的O.D.值為1.641。此外，以FT-IR光譜證實金奈米粒子膠體溶液的形成如圖7A所示。 Finally, in step (c), the aforementioned gold nanoparticles were dispersed in the double-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (200 mg, 1.0 mmol) as a medium, and the solution was Heating at 70 ° C for 10 minutes gave a colloidal solution of gold nanoparticles, as shown in Fig. 6, which had a λ max of 525 nm in the UV-Vis spectrum and an OD value of 1.641. Further, the formation of the colloidal solution of the gold nanoparticles by FT-IR spectroscopy was confirmed as shown in Fig. 7A.

實施例16 使用乳酸乙酯作為還原劑和檸檬酸做為分散劑而不加熱分散以合成金奈米粒子膠體溶液 Example 16 Using ethyl lactate as a reducing agent and citric acid as a dispersing agent without heat dispersion to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和乳酸乙酯(23.6毫克，0.20毫莫耳)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and ethyl lactate (23.6 mg, 0.20 mmol) were added to a 100 ml two-necked flat-bottomed flask and mixed into a mixed solution. .

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱12分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 12 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(200毫克，1.0毫莫耳)的水溶液50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以30℃加熱10分鐘，得到一金奈米粒子膠體溶液，其UV-Vis光譜中的λmax為525nm且其所測得的O.D.值為2.148。 Finally, in step (c), the aforementioned gold nanoparticles were dispersed in the double-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (200 mg, 1.0 mmol) as a medium, and the solution was Heating at 30 ° C for 10 minutes gave a colloidal solution of gold nanoparticles having a λ max of 525 nm in the UV-Vis spectrum and an OD value of 2.148.

實施例17 使用乳酸乙酯和乳酸作為組合還原劑以合成金奈米粒子膠體溶液 Example 17 Using ethyl lactate and lactic acid as a combined reducing agent to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和乳酸乙酯(11.6毫克，0.10毫莫耳)及乳酸(11.3毫克，0.13毫莫耳)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and ethyl lactate (11.6 mg, 0.10 mmol) and lactic acid (11.3 mg, 0.13 mmol) were added to 100. A two-neck flat-bottomed flask of cc was mixed and mixed into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱8.5分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 8.5 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(200毫克，1.0毫莫耳)的水溶液50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，其UV-Vis光譜中的λmax為530nm且其所測得的O.D.值為1.996。 Finally, in step (c), the aforementioned gold nanoparticles were dispersed in the double-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (200 mg, 1.0 mmol) as a medium, and the solution was Heating at 70 ° C for 10 minutes gave a colloidal solution of gold nanoparticles having a λ max of 530 nm in the UV-Vis spectrum and an OD value of 1.996.

實施例18 使用乳酸乙酯和1,4-丁二醇作為組合還原劑以合成金奈米粒子膠體溶液 Example 18 Using ethyl lactate and 1,4-butanediol as a combined reducing agent to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和乳酸乙酯(11.5毫克，0.10毫莫耳)及1,4-丁二醇(10.6毫克，0.12毫莫耳)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and ethyl lactate (11.5 mg, 0.10 mmol) and 1,4-butanediol (10.6 mg, 0.12) Millions of a two-neck flat-bottomed flask were added and mixed into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱12分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 12 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(200毫克，1.0毫莫耳)的水溶液50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，其UV-Vis光譜中的λmax為530nm且其所測得的O.D.值為1.017。 Finally, in step (c), the aforementioned gold nanoparticles were dispersed in the double-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (200 mg, 1.0 mmol) as a medium, and the solution was Heating at 70 ° C for 10 minutes gave a colloidal solution of gold nanoparticles having a λ max of 530 nm in the UV-Vis spectrum and an OD value of 1.017.

實施例19 使用乳酸乙酯和檸檬酸作為組合還原劑以合成金奈米粒子膠體溶液 Example 19 Using ethyl lactate and citric acid as a combined reducing agent to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和乳酸乙酯(17.2毫克，0.15毫莫耳)及檸檬酸(20.9毫克，0.11毫莫耳)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and ethyl lactate (17.2 mg, 0.15 mmol) and citric acid (20.9 mg, 0.11 mmol) were added. A 100 ml two-necked flat-bottomed flask was mixed and mixed into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱10.5分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 10.5 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(200毫克，1.0毫莫耳)的水溶液50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，其UV-Vis光譜中的λmax為525nm且其所測得的O.D.值為2.324。 Finally, in step (c), the aforementioned gold nanoparticles were dispersed in the double-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (200 mg, 1.0 mmol) as a medium, and the solution was Heating at 70 ° C for 10 minutes gave a colloidal solution of gold nanoparticles having a λ max of 525 nm in the UV-Vis spectrum and an OD value of 2.324.

實施例20 使用乳酸乙酯和PEG800作為組合還原劑以合成金奈米粒子膠體溶液 Example 20 Using ethyl lactate and PEG 800 as a combined reducing agent to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和乳酸乙酯(12.2毫克，0.10毫莫耳)及PEG800(81.4毫克)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and ethyl lactate (12.2 mg, 0.10 mmol) and PEG 800 (81.4 mg) were added to a 100 ml double neck flat bottom. The flasks were mixed and mixed into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱20分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 20 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(200毫克，1.0毫莫耳)的水溶液50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，其UV-Vis光譜中的λmax為530nm且其所測得的O.D.值為3.802。 Finally, in step (c), the aforementioned gold nanoparticles were dispersed in the double-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (200 mg, 1.0 mmol) as a medium, and the solution was Heating at 70 ° C for 10 minutes gave a colloidal solution of gold nanoparticles having a λ max of 530 nm in the UV-Vis spectrum and an OD value of 3.802.

實施例21 使用乳酸乙酯和PEG1000作為組合還原劑以合成金奈米粒子膠體溶液 Example 21 Using ethyl lactate and PEG1000 as a combined reducing agent to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和乳酸乙酯(14.0毫克，0.12毫莫耳)及PEG1000(103毫克)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and ethyl lactate (14.0 mg, 0.12 mmol) and PEG 1000 (103 mg) were added to a 100 ml double neck flat bottom. The flasks were mixed and mixed into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱20分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 20 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(200毫克，1.0毫莫耳)的水溶液50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，其UV-Vis光譜中的λmax為525nm且其所測得的O.D.值為3.086。 Finally, in step (c), the aforementioned gold nanoparticles were dispersed in the double-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (200 mg, 1.0 mmol) as a medium, and the solution was Heating at 70 ° C for 10 minutes gave a colloidal solution of gold nanoparticles having a λ max of 525 nm in the UV-Vis spectrum and an OD value of 3.086.

實施例22 使用乳酸乙酯和PEG4000作為組合還原劑以合成金奈米粒子膠體溶液 Example 22 Using ethyl lactate and PEG4000 as a combined reducing agent to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和乳酸乙酯(12.9毫克，0.11毫莫耳)及PEG4000(402.8毫克)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and ethyl lactate (12.9 mg, 0.11 mmol) and PEG 4000 (402.8 mg) were added to a 100 ml double neck flat bottom. The flasks were mixed and mixed into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱30分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 30 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(200毫克，1.0毫莫耳)的水溶液50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，其UV-Vis光譜中的λmax為530nm且其所測得的O.D.值為3.012。 Finally, in step (c), the aforementioned gold nanoparticles were dispersed in the double-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (200 mg, 1.0 mmol) as a medium, and the solution was Heating at 70 ° C for 10 minutes gave a colloidal solution of gold nanoparticles having a λ max of 530 nm in the UV-Vis spectrum and an OD value of 3.012.

實施例23 使用乳酸乙酯和PEG8000作為組合還原劑以合成金奈米粒子膠體溶液 Example 23 Using ethyl lactate and PEG 8000 as a combined reducing agent to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和乳酸甲酯(11毫克，0.09毫莫耳)及PEG8000(807.5毫克)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and methyl lactate (11 mg, 0.09 mmol) and PEG 8000 (807.5 mg) were added to a 100 ml double neck flat bottom. The flasks were mixed and mixed into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱30分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 30 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(200毫克，1.0毫莫耳)的水溶液50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，如圖8所示，其在UV-Vis光譜中的λmax為535nm且其所測得的O.D.值為3.1。此外，如圖9的TEM影像所示，該金奈米粒子之平均粒徑為33nm至34nm。 Finally, in step (c), the aforementioned gold nanoparticles were dispersed in the double-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (200 mg, 1.0 mmol) as a medium, and the solution was Heating at 70 ° C for 10 minutes gave a colloidal solution of gold nanoparticles, as shown in Fig. 8, which had a λ max of 535 nm in the UV-Vis spectrum and an OD value of 3.1. Further, as shown in the TEM image of FIG. 9, the average particle diameter of the gold nanoparticles is from 33 nm to 34 nm.

實施例24 使用乳酸乙酯和PEG10000作為組合還原劑以合成金奈米粒子膠體溶液 Example 24 Using ethyl lactate and PEG 10000 as a combined reducing agent to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和乳酸乙酯(12.1毫克，0.10毫莫耳)及PEG10000(1.005克)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and ethyl lactate (12.1 mg, 0.10 mmol) and PEG 10000 (1.005 g) were added to a 100 ml double neck flat bottom. The flasks were mixed and mixed into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱30分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 30 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(200毫克，1.0毫莫耳)的水溶液50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，其UV-Vis光譜中的λ max為530nm且其所測得的O.D.值為2.882。 Finally, in step (c), the aforementioned gold nanoparticles were dispersed in the double-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (200 mg, 1.0 mmol) as a medium, and the solution was Heating at 70 ° C for 10 minutes gave a colloidal solution of gold nanoparticles having a λ max of 530 nm in the UV-Vis spectrum and an OD value of 2.882.

實施例25 使用乳酸乙酯和PEG11000作為組合還原劑以合成金奈米粒子膠體溶液 Example 25 Using ethyl lactate and PEG 11000 as a combined reducing agent to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和乳酸乙酯(12.5毫克，0.11毫莫耳)及PEG11000(1.07克)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and ethyl lactate (12.5 mg, 0.11 mmol) and PEG 11000 (1.07 g) were added to a 100 ml double neck flat bottom. The flasks were mixed and mixed into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱30分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 30 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(200毫克，1.0毫莫耳)的水溶液50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，其UV-Vis光譜中的λ max為540nm且其所測得的O.D.值為2.996。 Finally, in step (c), the aforementioned gold nanoparticles were dispersed in the double-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (200 mg, 1.0 mmol) as a medium, and the solution was Heating at 70 ° C for 10 minutes gave a colloidal solution of gold nanoparticles having a λ max of 540 nm in the UV-Vis spectrum and an OD value of 2.996.

實施例26 使用γ-丁內酯作為還原劑和氫氧化鈉做為分散劑以合成金奈米粒子膠體溶液 Example 26 Using γ-butyrolactone as a reducing agent and sodium hydroxide as a dispersing agent to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和γ-丁內酯(18.4毫克，0.21毫莫耳)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and γ-butyrolactone (18.4 mg, 0.21 mmol) were added to a 100 ml two-necked flat-bottomed flask and mixed into one. mixture.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱15分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 15 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有氫氧化鈉(46.5毫克，1.2毫莫耳)的水溶液50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，其UV-Vis光譜中的λmax為565nm且其所測得的O.D.值為0.134。 Finally, in step (c), the aforementioned gold nanoparticles are dispersed in the two-necked flat-bottomed flask using 50 ml of an aqueous solution containing sodium hydroxide (46.5 mg, 1.2 mmol) as a medium, and The solution was heated at 70 ° C for 10 minutes to obtain a gold nanoparticle colloidal solution having a λ max of 565 nm in the UV-Vis spectrum and an OD value of 0.134.

實施例27 使用γ-丁內酯作為還原劑和檸檬酸做為分散劑以合成金奈米粒子膠體溶液 Example 27 Using γ-butyrolactone as a reducing agent and citric acid as a dispersing agent to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和γ-丁內酯(19.3毫克，0.22毫莫耳)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and γ-butyrolactone (19.3 mg, 0.22 mmol) were added to a 100 ml two-necked flat-bottomed flask and mixed into one. mixture.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱12分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 12 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(200毫克，1.0毫莫耳)的水溶液50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，如圖10所示，其在UV-Vis光譜中的λmax為530nm且其以稀釋50%的稀釋液量測反推得知O.D.值為2.866。此外，以FT-IR光譜證實金奈米粒子膠體溶液的形成如圖11A所示。而如圖12的TEM影像所示，該金奈米粒子之平均粒徑為27nm至28nm。 Finally, in step (c), the aforementioned gold nanoparticles were dispersed in the double-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (200 mg, 1.0 mmol) as a medium, and the solution was Heating at 70 ° C for 10 minutes, a gold nanoparticle colloidal solution was obtained, as shown in FIG. 10, its λ max in the UV-Vis spectrum was 530 nm and it was inversely deduced by the dilution of 50%. The value is 2.866. Further, the formation of the colloidal solution of the gold nanoparticles by FT-IR spectroscopy was confirmed as shown in Fig. 11A. As shown in the TEM image of FIG. 12, the average particle diameter of the gold nanoparticles is from 27 nm to 28 nm.

實施例28 使用γ-丁內酯作為還原劑和檸檬酸做為分散劑而加熱至50℃分散以合成金奈米粒子膠體溶液 Example 28 Using γ-butyrolactone as a reducing agent and citric acid as a dispersing agent and heating to 50 ° C to disperse to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和γ-丁內酯(17.2毫克，0.20毫莫耳)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and γ-butyrolactone (17.2 mg, 0.20 mmol) were added to a 100 ml two-necked flat-bottomed flask and mixed into one. mixture.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱12分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 12 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(200毫克，1.0毫莫耳)的水溶液50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以 50℃加熱10分鐘，得到一金奈米粒子膠體溶液，其UV-Vis光譜中的λmax為525nm且其所測得的O.D.值為2.29。 Finally, in step (c), the aforementioned gold nanoparticles were dispersed in the double-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (200 mg, 1.0 mmol) as a medium, and the solution was Heating at 50 ° C for 10 minutes gave a colloidal solution of gold nanoparticles having a λ max of 525 nm in the UV-Vis spectrum and an OD value of 2.29.

實施例29 使用γ-丁內酯和乳酸作為組合還原劑以合成金奈米粒子膠體溶液 Example 29 Using γ-butyrolactone and lactic acid as a combined reducing agent to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和γ-丁內酯(10.2毫克，0.12毫莫耳)及乳酸(11.3毫克，0.13毫莫耳)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and γ-butyrolactone (10.2 mg, 0.12 mmol) and lactic acid (11.3 mg, 0.13 mmol) A 100 ml two-necked flat-bottomed flask was added and mixed into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱18分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 18 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(200毫克，1.0毫莫耳)的水溶液50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，其UV-Vis光譜中的λmax為525nm且其所測得的O.D.值為1.582。 Finally, in step (c), the aforementioned gold nanoparticles were dispersed in the double-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (200 mg, 1.0 mmol) as a medium, and the solution was Heating at 70 ° C for 10 minutes gave a colloidal solution of gold nanoparticles having a λ max of 525 nm in the UV-Vis spectrum and an OD value of 1.582.

實施例30 使用γ-丁內酯和乳酸甲酯作為組合還原劑以合成金奈米粒子膠體溶液 Example 30 Using γ-butyrolactone and methyl lactate as a combined reducing agent to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和γ-丁內酯(11.9毫克，0.14毫莫耳)及乳酸甲酯(11.3毫克，0.11毫莫耳)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and γ-butyrolactone (11.9 mg, 0.14 mmol) and methyl lactate (11.3 mg, 0.11 mmol) Ears) A 100 ml two-necked flat-bottomed flask was added and mixed into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱17分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前 述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 17 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. Before proceeding While the reduction reaction was being carried out, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(200毫克，1.0毫莫耳)的水溶液50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，其UV-Vis光譜中的λmax為525nm且其所測得的O.D.值為0.463。 Finally, in step (c), the aforementioned gold nanoparticles were dispersed in the double-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (200 mg, 1.0 mmol) as a medium, and the solution was Heating at 70 ° C for 10 minutes gave a colloidal solution of gold nanoparticles having a λ max of 525 nm in the UV-Vis spectrum and an OD value of 0.463.

實施例31 使用γ-丁內酯和乳酸甲酯作為組合還原劑於短的反應時間下以合成金奈米粒子膠體溶液 Example 31 Using γ-butyrolactone and methyl lactate as a combined reducing agent to synthesize a colloidal solution of gold nanoparticles in a short reaction time

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和γ-丁內酯(11.9毫克，0.14毫莫耳)及乳酸甲酯(11.3毫克，0.11毫莫耳)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and γ-butyrolactone (11.9 mg, 0.14 mmol) and methyl lactate (11.3 mg, 0.11 mmol) Ears) A 100 ml two-necked flat-bottomed flask was added and mixed into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱12分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。最後，在步驟(c)中，使用含有檸檬酸(200毫克，1.0毫莫耳)的水溶液50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，其UV-Vis光譜中的λmax為525nm且其所測得的O.D.值為1.496。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 12 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection. Finally, in step (c), the aforementioned gold nanoparticles were dispersed in the double-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (200 mg, 1.0 mmol) as a medium, and the solution was Heating at 70 ° C for 10 minutes gave a colloidal solution of gold nanoparticles having a λ max of 525 nm in the UV-Vis spectrum and an OD value of 1.496.

實施例32 使用γ-丁內酯和乳酸乙酯作為組合還原劑以合成金奈米粒子膠體溶液 Example 32 Using γ-butyrolactone and ethyl lactate as a combined reducing agent to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和γ-丁內酯(11.1毫克，0.13毫莫耳)及乳酸乙酯(12.2毫克，0.10毫莫耳)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and γ-butyrolactone (11.1 mg, 0.13 mmol) and ethyl lactate (12.2 mg, 0.10 mmol) Ears) A 100 ml two-necked flat-bottomed flask was added and mixed into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱12分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 12 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(200毫克，1.0毫莫耳)的水溶液50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，其UV-Vis光譜中的λmax為525nm且其所測得的O.D.值為1.416。 Finally, in step (c), the aforementioned gold nanoparticles were dispersed in the double-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (200 mg, 1.0 mmol) as a medium, and the solution was Heating at 70 ° C for 10 minutes gave a colloidal solution of gold nanoparticles having a λ max of 525 nm in the UV-Vis spectrum and an OD value of 1.416.

實施例33 使用聚乳酸作為還原劑以合成金奈米粒子膠體溶液 Example 33 Using polylactic acid as a reducing agent to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和聚乳酸(PLA)(90.6毫克)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in the step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and polylactic acid (PLA) (90.6 mg) were placed in a 100 ml two-necked flat-bottomed flask and mixed into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱12分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 12 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(200毫克，1.0毫莫耳)的水溶液50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，如圖13所示，其在UV-Vis光譜中的λmax為525nm且其以稀釋50%的稀釋液所測得的O.D.值為2.426。此外，以FT-IR光譜證實金奈米粒子膠體溶液的形成如圖14A所示。 Finally, in step (c), the aforementioned gold nanoparticles were dispersed in the double-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (200 mg, 1.0 mmol) as a medium, and the solution was Heating at 70 ° C for 10 minutes gave a colloidal solution of gold nanoparticles, as shown in Figure 13, its λ max in the UV-Vis spectrum was 525 nm and its OD value measured by diluting 50% of the dilution was 2.426. Further, the formation of the colloidal solution of the gold nanoparticles by FT-IR spectroscopy was confirmed as shown in Fig. 14A.

實施例34 使用聚乳酸作為還原劑且反應之加熱溫度為50℃以合成金奈米粒子膠體溶液 Example 34 Using polylactic acid as a reducing agent and heating at a reaction temperature of 50 ° C to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和聚乳酸(90.8毫克)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in the step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and polylactic acid (90.8 mg) were placed in a 100 ml two-necked flat-bottomed flask and mixed to form a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於60℃加熱12分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、小於前述混合溶液20體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 60 ° C for 12 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, which is less than 20% by volume of the mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(200毫克，1.0毫莫耳)的水溶液50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，其UV-Vis光譜中的λmax為525nm且其所測得的O.D.值為2.444。 Finally, in step (c), the aforementioned gold nanoparticles were dispersed in the double-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (200 mg, 1.0 mmol) as a medium, and the solution was Heating at 70 ° C for 10 minutes gave a colloidal solution of gold nanoparticles having a λ max of 525 nm in the UV-Vis spectrum and an OD value of 2.444.

實施例35 使用乙醇酸作為還原劑以合成金奈米粒子膠體溶液 Example 35 Using Glycolic Acid as a Reducing Agent to Synthesize a Gold Nanoparticle Colloidal Solution

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和乙醇酸(19.1毫克，0.25毫莫耳)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in the step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and glycolic acid (19.1 mg, 0.25 mmol) were placed in a 100 ml two-necked flat-bottomed flask and mixed to form a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱15分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 15 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(200毫克，1.0毫莫耳)的水溶液50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，如圖15所示，其在UV-Vis光譜中的λmax為535nm且其以稀釋50%的稀釋液量測反推得知O.D.值為5.226。 Finally, in step (c), the aforementioned gold nanoparticles were dispersed in the double-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (200 mg, 1.0 mmol) as a medium, and the solution was Heating at 70 ° C for 10 minutes, a gold nanoparticle colloidal solution was obtained, as shown in FIG. 15 , which had a λ max of 535 nm in the UV-Vis spectrum and was inversely estimated by the dilution of 50%. The value is 5.226.

實施例36 使用乳酸作為還原劑和分散劑以合成金奈米粒子膠體溶液 Example 36 Using lactic acid as a reducing agent and dispersing agent to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和乳酸(20.4毫克，0.23毫莫耳)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in the step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and lactic acid (20.4 mg, 0.23 mmol) were placed in a 100 ml two-necked flat-bottomed flask and mixed into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱15分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 15 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有乳酸(220毫克，2.4毫莫耳)的水溶液50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，其UV-Vis光譜中的λmax為535nm且其所測得的O.D.值為0.897。 Finally, in step (c), 50 ml of an aqueous solution containing lactic acid (220 mg, 2.4 mmol) was used as a medium, and the aforementioned gold nanoparticles were dispersed in the two-necked flat-bottomed flask, and the solution was Heating at 70 ° C for 10 minutes gave a colloidal solution of gold nanoparticles having a λ max of 535 nm in the UV-Vis spectrum and an OD value of 0.897.

實施例37 使用乳酸作為還原劑和檸檬酸做為分散劑以合成金奈米粒子膠體溶液 Example 37 Using lactic acid as a reducing agent and citric acid as a dispersing agent to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和乳酸(21.3毫克，0.24毫莫耳)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in the step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and lactic acid (21.3 mg, 0.24 mmol) were placed in a 100 ml two-necked flat-bottomed flask and mixed into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱9分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 9 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(200毫克，1.0毫莫耳)的水溶液50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以 70℃加熱10分鐘，得到一金奈米粒子膠體溶液，如圖16所示，其在UV-Vis光譜中的λmax為525nm且其以稀釋50%的稀釋液量測反推得知O.D.值為2.468。此外，以FT-IR光譜證實金奈米粒子膠體溶液的形成如圖17A所示。並且，如圖18所示，該金奈米粒子膠體溶液的界達電位為-44.86mV。 Finally, in step (c), the aforementioned gold nanoparticles were dispersed in the double-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (200 mg, 1.0 mmol) as a medium, and the solution was After heating at 70 ° C for 10 minutes, a gold nanoparticle colloidal solution was obtained, as shown in FIG. 16 , which had a λ max of 525 nm in the UV-Vis spectrum and was inversely estimated by the dilution of 50%. The value is 2.468. Further, the formation of the colloidal solution of the gold nanoparticles by FT-IR spectroscopy was confirmed as shown in Fig. 17A. Further, as shown in Fig. 18, the boundary potential of the colloidal solution of the gold nanoparticles was -44.86 mV.

實施例38 使用檸檬酸作為還原劑以合成金奈米粒子膠體溶液 Example 38 Using citric acid as a reducing agent to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和檸檬酸(40.3毫克，0.21毫莫耳)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in the step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and citric acid (40.3 mg, 0.21 mmol) were placed in a 100 ml two-necked flat-bottomed flask and mixed into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱12分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 12 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用純水50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，如圖19所示，其在UV-Vis光譜中的λmax為525nm且其所測得的O.D.值為2.412。 Finally, in the step (c), 50 ml of pure water was used as a medium, and the aforementioned gold nanoparticles were dispersed in the double-necked flat-bottomed flask, and the solution was heated at 70 ° C for 10 minutes to obtain a gold nanometer. The particle colloidal solution, as shown in Figure 19, had a λ max of 525 nm in the UV-Vis spectrum and an OD value of 2.412.

實施例39 使用檸檬酸作為還原劑以大規模合成金奈米粒子膠體溶液 Example 39 Large-scale synthesis of a colloidal solution of gold nanoparticles using citric acid as a reducing agent

首先，在步驟(a)中，將HAuCl4(0.2M水溶液10毫升，2毫莫耳)和檸檬酸(1.6克，83.4毫莫耳)加入2升的雙頸平底燒瓶並混合成一混合溶液。 First, in the step (a), HAuCl 4 (0.2 M aqueous solution 10 ml, 2 mmol) and citric acid (1.6 g, 83.4 mmol) were placed in a 2-liter two-necked flat-bottomed flask and mixed to form a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱14分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前 述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 14 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. Before proceeding While the reduction reaction was being carried out, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用純水2升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱30分鐘，得到一金奈米粒子膠體溶液，其UV-Vis光譜中的λmax為525nm且其所測得的O.D.值為2.433。 Finally, in the step (c), 2 liters of pure water was used as a medium, the aforementioned gold nanoparticles were dispersed in the two-necked flat-bottomed flask, and the solution was heated at 70 ° C for 30 minutes to obtain a gold nanometer. The particle colloidal solution had a λ max in the UV-Vis spectrum of 525 nm and an OD value of 2.433 as measured.

實施例40 使用檸檬酸作為還原劑和甘油做為分散劑以合成金奈米粒子膠體溶液 Example 40 Using citric acid as a reducing agent and glycerin as a dispersing agent to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.5毫升，0.1毫莫耳)和檸檬酸(80.8毫克，0.42毫莫耳)加入150毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in the step (a), HAuCl 4 (0.2 M aqueous solution 0.5 ml, 0.1 mmol) and citric acid (80.8 mg, 0.42 mmol) were placed in a 150 ml two-necked flat-bottomed flask and mixed into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱12分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 12 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有甘油(400毫克，4.3毫莫耳)的水溶液100毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，其UV-Vis光譜中的λmax為525nm且其所測得的O.D.值為2.472。 Finally, in step (c), 100 ml of an aqueous solution containing glycerol (400 mg, 4.3 mmol) was used as a medium, and the aforementioned gold nanoparticles were dispersed in the two-necked flat-bottomed flask, and the solution was Heating at 70 ° C for 10 minutes gave a colloidal solution of gold nanoparticles having a λ max of 525 nm in the UV-Vis spectrum and an OD value of 2.472 as measured.

實施例41 使用檸檬酸作為還原劑和PEG做為分散劑以合成金奈米粒子膠體溶液 Example 41 Using citric acid as a reducing agent and PEG as a dispersing agent to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.5毫升，0.1毫莫耳)和檸檬酸(81.3毫克，0.42毫莫耳)加入150毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in the step (a), HAuCl 4 (0.2 M aqueous solution 0.5 ml, 0.1 mmol) and citric acid (81.3 mg, 0.42 mmol) were placed in a 150 ml two-necked flat-bottomed flask and mixed into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱12分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個 金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 12 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The aforementioned reduction reaction produces a plurality of The gold nanoparticles, almost 0% by volume of the residue of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有PEG800(400毫克)的水溶液100毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，其UV-Vis光譜中的λmax為525nm且其所測得的O.D.值為2.13。 Finally, in step (c), the aforementioned gold nanoparticles were dispersed in the double-necked flat-bottomed flask using 100 ml of an aqueous solution containing PEG 800 (400 mg) as a medium, and the solution was heated at 70 ° C for 10 minutes. A gold nanoparticle colloidal solution having a λ max in the UV-Vis spectrum of 525 nm and an OD value of 2.13 was obtained.

實施例42 使用檸檬酸作為還原劑且加熱至150℃以合成金奈米粒子膠體溶液 Example 42 Using citric acid as a reducing agent and heating to 150 ° C to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和檸檬酸(40.2毫克，0.21毫莫耳)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in the step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and citric acid (40.2 mg, 0.21 mmol) were placed in a 100 ml two-necked flat-bottomed flask and mixed to form a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於150℃加熱2分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 150 ° C for 2 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用純水50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，其UV-Vis光譜中的λmax為525nm且其所測得的O.D.值為1.961。 Finally, in the step (c), 50 ml of pure water was used as a medium, and the aforementioned gold nanoparticles were dispersed in the double-necked flat-bottomed flask, and the solution was heated at 70 ° C for 10 minutes to obtain a gold nanometer. The particle colloidal solution had a λ max of 525 nm in the UV-Vis spectrum and its measured OD value was 1.961.

實施例43 使用檸檬酸作為還原劑且加熱至70℃以合成金奈米粒子膠體溶液 Example 43 Using citric acid as a reducing agent and heating to 70 ° C to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和檸檬酸(40.2毫克，0.21毫莫耳)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in the step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and citric acid (40.2 mg, 0.21 mmol) were placed in a 100 ml two-necked flat-bottomed flask and mixed to form a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於70℃加熱40分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、少於前述混合溶液20體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 70 ° C for 40 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The above reduction reaction produces a residue containing a plurality of gold nanoparticles, less than 20% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用純水50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，其UV-Vis光譜中的λmax為525nm且其所測得的O.D.值為2.492。 Finally, in the step (c), 50 ml of pure water was used as a medium, and the aforementioned gold nanoparticles were dispersed in the double-necked flat-bottomed flask, and the solution was heated at 70 ° C for 10 minutes to obtain a gold nanometer. The particle colloidal solution had a λ max of 525 nm in the UV-Vis spectrum and an OD value of 2.492.

實施例44 使用纖維素作為還原劑以合成金奈米粒子膠體溶液 Example 44 Using cellulose as a reducing agent to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和纖維素(40.8毫克)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in the step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and cellulose (40.8 mg) were placed in a 100 ml two-necked flat-bottomed flask and mixed into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱15分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 15 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(200毫克，1.0毫莫耳)的水溶液50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，如圖20所示，其在UV-Vis光譜中的λmax為530nm且其以稀釋50%的稀釋液量測反推得知O.D.值為4.17。 Finally, in step (c), the aforementioned gold nanoparticles were dispersed in the double-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (200 mg, 1.0 mmol) as a medium, and the solution was Heating at 70 ° C for 10 minutes, a gold nanoparticle colloidal solution was obtained, as shown in Figure 20, its λ max in the UV-Vis spectrum was 530 nm and it was inversely deduced to obtain OD by dilution of 50% dilution. The value is 4.17.

實施例45 使用羧甲基纖維素作為還原劑以合成金奈米粒子膠體溶液 Example 45 Using carboxymethylcellulose as a reducing agent to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和羧甲基纖維素(40毫克)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in the step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and carboxymethyl cellulose (40 mg) were placed in a 100 ml two-necked flat-bottomed flask and mixed into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱12分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 12 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(200毫克，1.0毫莫耳)的水溶液50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，如圖21所示，其在UV-Vis光譜中的λmax為530nm且其以稀釋50%的稀釋液量測反推得知O.D.值為3.528。 Finally, in step (c), the aforementioned gold nanoparticles were dispersed in the double-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (200 mg, 1.0 mmol) as a medium, and the solution was Heating at 70 ° C for 10 minutes, a gold nanoparticle colloidal solution was obtained, as shown in FIG. 21, its λ max in the UV-Vis spectrum was 530 nm and it was inversely deduced to obtain OD by dilution of 50% of the dilution. The value is 3.528.

實施例46 使用殼多醣作為還原劑以合成金奈米粒子膠體溶液 Example 46 Using chitin as a reducing agent to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和殼多醣(41.6毫克)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in the step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and chitin (41.6 mg) were placed in a 100 ml two-necked flat-bottomed flask and mixed into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱15分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 15 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(200毫克，1.0毫莫耳)的水溶液50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，如圖22所示，其在UV-Vis光譜中的λmax為567nm且其所測得的O.D.值為0.216。 Finally, in step (c), the aforementioned gold nanoparticles were dispersed in the double-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (200 mg, 1.0 mmol) as a medium, and the solution was Heating at 70 ° C for 10 minutes gave a colloidal solution of gold nanoparticles, as shown in Fig. 22, which had a λ max of 567 nm in the UV-Vis spectrum and an OD value of 0.216.

實施例47 使用殼聚醣作為還原劑以合成金奈米粒子膠體溶液 Example 47 Using chitosan as a reducing agent to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和殼聚醣(81.6毫克)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in the step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and chitosan (81.6 mg) were placed in a 100 ml two-necked flat-bottomed flask and mixed into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱15分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 15 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(200毫克，1.0毫莫耳)的水溶液50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，如圖23所示，其在UV-Vis光譜中的λmax為538nm且其所測得的O.D.值為0.162。此外，如圖24的TEM影像所示，該金奈米粒子之平均粒徑為38nm至39nm。然而，該金奈米粒子的形狀及尺寸並不均勻。 Finally, in step (c), the aforementioned gold nanoparticles were dispersed in the double-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (200 mg, 1.0 mmol) as a medium, and the solution was Heating at 70 ° C for 10 minutes gave a colloidal solution of gold nanoparticles, as shown in Fig. 23, which had a λ max of 538 nm in the UV-Vis spectrum and an OD value of 0.162. Further, as shown in the TEM image of FIG. 24, the average particle diameter of the gold nanoparticles is from 38 nm to 39 nm. However, the shape and size of the gold nanoparticles are not uniform.

實施例48 使用聚乙烯吡咯烷酮作為還原劑和分散劑以合成金奈米粒子膠體溶液 Example 48 Using polyvinylpyrrolidone as a reducing agent and dispersing agent to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和聚乙烯吡咯烷酮(48.5毫克)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in the step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and polyvinylpyrrolidone (48.5 mg) were placed in a 100 ml two-necked flat-bottomed flask and mixed to form a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於150℃加熱80分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 150 ° C for 80 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有聚乙烯吡咯烷酮(200毫克)的水溶液50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以60℃加熱10分鐘，得到一金奈米粒子膠體溶液，其顯示UV-Vis光譜中的λmax為535nm且其O.D.值為2.76。 Finally, in the step (c), 50 ml of an aqueous solution containing polyvinylpyrrolidone (200 mg) was used as a medium, and the aforementioned gold nanoparticles were dispersed in the two-necked flat-bottomed flask, and the solution was heated at 60 ° C. At 10 minutes, a gold nanoparticle colloidal solution was obtained which showed λ max in the UV-Vis spectrum of 535 nm and an OD value of 2.76.

實施例49 使用乳酸和1,4-丁二醇作為組合還原劑以合成金奈米粒子膠體溶液 Example 49 Using lactic acid and 1,4-butanediol as a combined reducing agent to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和乳酸(11.8毫克，0.13毫莫耳)及1,4-丁二醇(10.8毫克，0.12毫莫耳)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and lactic acid (11.8 mg, 0.13 mmol) and 1,4-butanediol (10.8 mg, 0.12 mmol) Ears) A 100 ml two-necked flat-bottomed flask was added and mixed into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱12分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 12 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(200毫克，1.0毫莫耳)的水溶液50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，其UV-Vis光譜中的λmax為530nm且其所測得的O.D.值為1.254。 Finally, in step (c), the aforementioned gold nanoparticles were dispersed in the double-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (200 mg, 1.0 mmol) as a medium, and the solution was Heating at 70 ° C for 10 minutes gave a colloidal solution of gold nanoparticles having a λ max of 530 nm in the UV-Vis spectrum and an OD value of 1.254.

實施例50 使用乳酸和檸檬酸作為組合還原劑以合成金奈米粒子膠體溶液 Example 50 Using lactic acid and citric acid as a combined reducing agent to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和乳酸(15.5毫克，0.17毫莫耳)及檸檬酸(20.3毫克，0.11毫莫耳)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and lactic acid (15.5 mg, 0.17 mmol) and citric acid (20.3 mg, 0.11 mmol) were added to 100 ml. The two-necked flat-bottomed flask was mixed and mixed into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱10.5分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 10.5 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(200毫克，1.0毫莫耳)的水溶液50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，其UV-Vis光譜中的λmax為525nm且其所測得的O.D.值為2.872。 Finally, in step (c), the aforementioned gold nanoparticles were dispersed in the double-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (200 mg, 1.0 mmol) as a medium, and the solution was Heating at 70 ° C for 10 minutes gave a colloidal solution of gold nanoparticles having a λ max of 525 nm in the UV-Vis spectrum and an OD value of 2.872.

實施例51 使用乳酸和PEG800作為組合還原劑以合成金奈米粒子膠體溶液 Example 51 Using lactic acid and PEG800 as a combined reducing agent to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和乳酸(11.3毫克，0.13毫莫耳)及PEG800(80.9毫克)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and lactic acid (11.3 mg, 0.13 mmol) and PEG 800 (80.9 mg) were added to a 100 ml two-necked flat-bottomed flask. Mix into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱17.5分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 17.5 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The above reduction reaction produces a residue containing gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(200毫克，1.0毫莫耳)的水溶液50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，其UV-Vis光譜中的λmax為525nm且其所測得的O.D.值為2.906。 Finally, in step (c), the aforementioned gold nanoparticles were dispersed in the double-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (200 mg, 1.0 mmol) as a medium, and the solution was Heating at 70 ° C for 10 minutes gave a colloidal solution of gold nanoparticles having a λ max of 525 nm in the UV-Vis spectrum and an OD value of 2.906.

實施例52 使用乳酸和PEG1000作為組合還原劑以合成金奈米粒子膠體溶液 Example 52 Using lactic acid and PEG1000 as a combined reducing agent to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和乳酸(11.2毫克，0.12毫莫耳)及PEG1000(101.9毫克)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and lactic acid (11.2 mg, 0.12 mmol) and PEG 1000 (101.9 mg) were added to a 100 ml two-necked flat-bottomed flask. Mix into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱17.5分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 17.5 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(200毫克，1.0毫莫耳)的水溶液50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，其UV-Vis光譜中的λmax為525nm且其所測得的O.D.值為2.996。 Finally, in step (c), the aforementioned gold nanoparticles were dispersed in the double-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (200 mg, 1.0 mmol) as a medium, and the solution was Heating at 70 ° C for 10 minutes gave a colloidal solution of gold nanoparticles having a λ max of 525 nm in the UV-Vis spectrum and an OD value of 2.996.

實施例53 使用乳酸和PEG4000作為組合還原劑以合成金奈米粒子膠體溶液 Example 53 Using lactic acid and PEG4000 as a combined reducing agent to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和乳酸(11.1毫克，0.12毫莫耳)及PEG4000(400.2毫克)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and lactic acid (11.1 mg, 0.12 mmol) and PEG 4000 (400.2 mg) were added to a 100 ml two-necked flat-bottomed flask. Mix into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱30分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 30 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(200毫克，1.0毫莫耳)的水溶液50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，其UV-Vis光譜中的λmax為525nm且其所測得的O.D.值為2.836。 Finally, in step (c), the aforementioned gold nanoparticles were dispersed in the double-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (200 mg, 1.0 mmol) as a medium, and the solution was Heating at 70 ° C for 10 minutes gave a colloidal solution of gold nanoparticles having a λ max of 525 nm in the UV-Vis spectrum and an OD value of 2.836.

實施例54 使用乳酸和PEG8000作為組合還原劑以合成金奈米粒子膠體溶液 Example 54 Using lactic acid and PEG 8000 as a combined reducing agent to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和乳酸(10.5毫克，0.12毫莫耳)及PEG8000(802.3毫克)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and lactic acid (10.5 mg, 0.12 mmol) and PEG 8000 (802.3 mg) were added to a 100 ml two-necked flat-bottomed flask. Mix into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱30分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 30 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(200毫克，1.0毫莫耳)的水溶液50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，其UV-Vis光譜中的λmax為535nm且其所測得的O.D.值為3.166。 Finally, in step (c), the aforementioned gold nanoparticles were dispersed in the double-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (200 mg, 1.0 mmol) as a medium, and the solution was Heating at 70 ° C for 10 minutes gave a colloidal solution of gold nanoparticles having a λ max of 535 nm in the UV-Vis spectrum and an OD value of 3.166.

實施例55 使用乳酸和PEG10000作為組合還原劑以合成金奈米粒子膠體溶液 Example 55 Using lactic acid and PEG 10000 as a combined reducing agent to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和乳酸(11.7毫克，0.13毫莫耳)及PEG10000(1.042克)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and lactic acid (11.7 mg, 0.13 mmol) and PEG 10000 (1.042 g) were added to a 100 ml two-necked flat-bottomed flask. Mix into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱30分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 30 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(200毫克，1.0毫莫耳)的水溶液50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，其UV-Vis光譜中的λmax為535nm且其所測得的O.D.值為3.12。 Finally, in step (c), the aforementioned gold nanoparticles were dispersed in the double-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (200 mg, 1.0 mmol) as a medium, and the solution was Heating at 70 ° C for 10 minutes gave a colloidal solution of gold nanoparticles having a λ max of 535 nm in the UV-Vis spectrum and an OD value of 3.12.

實施例56 使用乳酸和PEG11000作為組合還原劑以合成金奈米粒子膠體溶液 Example 56 Using lactic acid and PEG 11000 as a combined reducing agent to synthesize a colloidal solution of gold nanoparticles

首先，在步驟(a)中，將HAuCl4(0.2M水溶液0.25毫升，0.05毫莫耳)和乳酸(11.7毫克，0.13毫莫耳)及PEG11000(1.109克)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), HAuCl 4 (0.2 M aqueous solution 0.25 ml, 0.05 mmol) and lactic acid (11.7 mg, 0.13 mmol) and PEG 11000 (1.109 g) were added to a 100 ml two-necked flat-bottomed flask. Mix into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於130℃加熱30分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個金奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 130 ° C for 30 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The reduction reaction produces a residue containing a plurality of gold nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(200毫克，1.0毫莫耳)的水溶液50毫升作為介質，將前述的金奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一金奈米粒子膠體溶液，其UV-Vis光譜中的λmax為535nm且其所測得的O.D.值為3.282。 Finally, in step (c), the aforementioned gold nanoparticles were dispersed in the double-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (200 mg, 1.0 mmol) as a medium, and the solution was Heating at 70 ° C for 10 minutes gave a colloidal solution of gold nanoparticles having a λ max of 535 nm in the UV-Vis spectrum and an OD value of 3.282.

實施例57 使用乳酸甲酯作為還原劑以合成銀奈米粒子膠體溶液 Example 57 Using methyl lactate as a reducing agent to synthesize a silver nanoparticle colloidal solution

首先，在步驟(a)中，將AgNO3(0.1M水溶液0.1毫升，0.01毫莫耳)和乳酸甲酯(24.5毫克，0.24毫莫耳)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), AgNO 3 (0.1 M aqueous solution 0.1 ml, 0.01 mmol) and methyl lactate (24.5 mg, 0.24 mmol) were added to a 100 ml two-necked flat-bottomed flask and mixed into a mixed solution. .

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於150℃加熱12分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個銀奈米粒子、幾乎為前述混合溶液0體積%的殘餘物，以及二氧化氮氣體。在進 行前述還原反應的同時，將由還原反應所產生的二氧化氮氣體從連接至該雙頸平底燒瓶回收口的通道，導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 150 ° C for 12 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The above reduction reaction produces a residue containing a plurality of silver nanoparticles, almost 0% by volume of the aforementioned mixed solution, and a nitrogen dioxide gas. In progress While the foregoing reduction reaction was carried out, the nitrogen dioxide gas produced by the reduction reaction was led to a vial connected to the recovery port of the double-necked flat-bottomed flask to a conical flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(33.6毫克，0.17毫莫耳)及氫氧化鈉(46.5毫克，1.12毫莫耳)的水溶液50毫升作為介質，將前述的銀奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱15分鐘，得到一銀奈米粒子膠體溶液，其UV-Vis光譜中的λmax為390nm且其所測得的O.D.值為2.433。 Finally, in step (c), the aforementioned silver nanoparticles are dispersed using 50 ml of an aqueous solution containing citric acid (33.6 mg, 0.17 mmol) and sodium hydroxide (46.5 mg, 1.12 mmol) as a medium. In the two-necked flat-bottomed flask, the solution was heated at 70 ° C for 15 minutes to obtain a silver nanoparticle colloidal solution having a λ max of 390 nm in the UV-Vis spectrum and an OD value of 2.433. .

實施例58 使用乳酸甲酯和檸檬酸作為組合還原劑以合成銀奈米粒子膠體溶液 Example 58 Using methyl lactate and citric acid as a combined reducing agent to synthesize a silver nanoparticle colloidal solution

首先，在步驟(a)中，將AgNO3(0.1M水溶液0.1毫升，0.01毫莫耳)和檸檬酸(45.9毫克，0.24毫莫耳)及乳酸甲酯(11.4毫克，0.11毫莫耳)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), AgNO 3 (0.1 M aqueous solution 0.1 ml, 0.01 mmol) and citric acid (45.9 mg, 0.24 mmol) and methyl lactate (11.4 mg, 0.11 mmol) were added. A 100 ml two-necked flat-bottomed flask was mixed and mixed into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於150℃加熱12分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個銀奈米粒子、幾乎為前述混合溶液0體積%的殘餘物，以及二氧化氮氣體。在進行前述還原反應的同時，將還原反應中所產生的二氧化氮氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 150 ° C for 12 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The above reduction reaction produces a residue containing a plurality of silver nanoparticles, almost 0% by volume of the aforementioned mixed solution, and a nitrogen dioxide gas. While the aforementioned reduction reaction was carried out, the nitrogen dioxide gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(33.6毫克，0.17毫莫耳)及氫氧化鈉(46.5毫克，1.12毫莫耳)的水溶液50毫升作為介質，將前述的銀奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱15分鐘，得到一銀奈米粒子膠體溶液，如圖25所示，其在UV-Vis光譜中的λmax為390nm且以稀釋50%的稀釋液量測反推得知的O.D.值為2.882。此外，如圖26的TEM影像所示，該銀奈米粒子之平均粒徑為10nm至11nm。 Finally, in step (c), the aforementioned silver nanoparticles are dispersed using 50 ml of an aqueous solution containing citric acid (33.6 mg, 0.17 mmol) and sodium hydroxide (46.5 mg, 1.12 mmol) as a medium. In the two-necked flat-bottomed flask, the solution was heated at 70 ° C for 15 minutes to obtain a silver nanoparticle colloidal solution, as shown in FIG. 25, which had a λ max of 390 nm in the UV-Vis spectrum and was diluted. The OD value of the 50% dilution measurement was 2.882. Further, as shown in the TEM image of FIG. 26, the silver nanoparticles have an average particle diameter of 10 nm to 11 nm.

實施例59 使用乳酸乙酯和檸檬酸作為組合還原劑以合成銀奈米粒子膠體溶液 Example 59 Using ethyl lactate and citric acid as a combined reducing agent to synthesize a silver nanoparticle colloidal solution

首先，在步驟(a)中，將AgNO3(0.1M水溶液0.1毫升，0.01毫莫耳)和檸檬酸(45.9毫克，0.24毫莫耳)及乳酸乙酯(11.7毫克，0.10毫莫耳)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), AgNO 3 (0.1 M aqueous solution 0.1 ml, 0.01 mmol) and citric acid (45.9 mg, 0.24 mmol) and ethyl lactate (11.7 mg, 0.10 mmol) were added. A 100 ml two-necked flat-bottomed flask was mixed and mixed into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於150℃加熱12分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個銀奈米粒子、幾乎為前述混合溶液0體積%的殘餘物，以及二氧化氮氣體。在進行前述還原反應的同時，將還原反應中所產生的二氧化氮氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 150 ° C for 12 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The above reduction reaction produces a residue containing a plurality of silver nanoparticles, almost 0% by volume of the aforementioned mixed solution, and a nitrogen dioxide gas. While the aforementioned reduction reaction was carried out, the nitrogen dioxide gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(33.6毫克，0.17毫莫耳)及氫氧化鈉(46.5毫克，1.12毫莫耳)的水溶液50毫升作為介質，將前述的銀奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱15分鐘，得到一銀奈米粒子膠體溶液，如圖27所示，其在UV-Vis光譜中的λmax為390nm且以稀釋50%的稀釋液量測反推得知的O.D.值為2.812。 Finally, in step (c), the aforementioned silver nanoparticles are dispersed using 50 ml of an aqueous solution containing citric acid (33.6 mg, 0.17 mmol) and sodium hydroxide (46.5 mg, 1.12 mmol) as a medium. In the two-necked flat-bottomed flask, the solution was heated at 70 ° C for 15 minutes to obtain a silver nanoparticle colloidal solution, as shown in FIG. 27, which had a λ max of 390 nm in the UV-Vis spectrum and was diluted. The OD value of the 50% dilution measurement was 2.812.

實施例60 使用乳酸和檸檬酸作為組合還原劑以合成銀奈米粒子膠體溶液 Example 60 Using lactic acid and citric acid as a combined reducing agent to synthesize a silver nanoparticle colloidal solution

首先，在步驟(a)中，將AgNO3(0.1M水溶液0.1毫升，0.01毫莫耳)和檸檬酸(45.4毫克，0.24毫莫耳)及乳酸(10.3毫克，0.11毫莫耳)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), AgNO 3 (0.1 M aqueous solution 0.1 ml, 0.01 mmol) and citric acid (45.4 mg, 0.24 mmol) and lactic acid (10.3 mg, 0.11 mmol) were added to 100 ml. The two-necked flat-bottomed flask was mixed and mixed into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於150℃加熱12分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個銀奈米粒子、幾乎為前述混合溶液0體積%的殘餘物，以及二氧化氮氣體。在進行前述還原反應的同時，將還原反應中所產生的二氧化氮氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 150 ° C for 12 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The above reduction reaction produces a residue containing a plurality of silver nanoparticles, almost 0% by volume of the aforementioned mixed solution, and a nitrogen dioxide gas. While the aforementioned reduction reaction was carried out, the nitrogen dioxide gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(33.6毫克，0.17毫莫耳)及氫氧化鈉(46.5毫克，1.12毫莫耳)的水溶液50毫升作為介質，將前述的銀奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱15分鐘，得到一銀奈米粒子膠體溶液，如圖28所示，其在UV-Vis光譜中的λmax為390nm且以稀釋50%的稀釋液量測反推得知的O.D.值為2.798。 Finally, in step (c), the aforementioned silver nanoparticles are dispersed using 50 ml of an aqueous solution containing citric acid (33.6 mg, 0.17 mmol) and sodium hydroxide (46.5 mg, 1.12 mmol) as a medium. In the two-necked flat-bottomed flask, the solution was heated at 70 ° C for 15 minutes to obtain a silver nanoparticle colloidal solution, as shown in FIG. 28, which had a λ max of 390 nm in the UV-Vis spectrum and was diluted. The OD value of the 50% dilution measurement was 2.798.

實施例61 使用檸檬酸作為還原劑和分散劑以合成銀奈米粒子膠體溶液 Example 61 Using Citric Acid as a Reducing Agent and Dispersing Agent to Synthesize Silver Nanoparticle Colloidal Solution

首先，在步驟(a)中，將AgNO3(0.1M水溶液0.1毫升，0.01毫莫耳)和檸檬酸(45.1毫克，0.23毫莫耳)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in the step (a), AgNO 3 (0.1 M aqueous solution 0.1 ml, 0.01 mmol) and citric acid (45.1 mg, 0.23 mmol) were placed in a 100 ml two-necked flat-bottomed flask and mixed to form a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於150℃加熱12分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個銀奈米粒子、幾乎為前述混合溶液0體積%的殘餘物，以及二氧化氮氣體。在進行前述還原反應的同時，將還原反應中所產生的二氧化氮氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 150 ° C for 12 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The above reduction reaction produces a residue containing a plurality of silver nanoparticles, almost 0% by volume of the aforementioned mixed solution, and a nitrogen dioxide gas. While the aforementioned reduction reaction was carried out, the nitrogen dioxide gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(33.6毫克，0.17毫莫耳)及氫氧化鈉(46.5毫克，1.12毫莫耳)的水溶液50毫升作為介質，將前述的銀奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱10分鐘，得到一銀奈米粒子膠體溶液，如圖29所示，其在UV-Vis光譜中的λmax為390nm且以稀釋50%的稀釋液量測反推得知的O.D.值為2.602。 Finally, in step (c), the aforementioned silver nanoparticles are dispersed using 50 ml of an aqueous solution containing citric acid (33.6 mg, 0.17 mmol) and sodium hydroxide (46.5 mg, 1.12 mmol) as a medium. In the two-necked flat-bottomed flask, the solution was heated at 70 ° C for 10 minutes to obtain a silver nanoparticle colloidal solution, as shown in FIG. 29, which had a λ max of 390 nm in the UV-Vis spectrum and was diluted. The OD value of the 50% dilution measurement was 2.602.

實施例62 使用乳酸乙酯作為還原劑以合成鈀奈米粒子膠體溶液 Example 62 Using ethyl lactate as a reducing agent to synthesize a palladium nanoparticle colloidal solution

首先，在步驟(a)中，將PdCl2(0.1M水溶液0.1毫升，0.01毫莫耳)和乳酸乙酯(27.8毫克，0.24毫莫耳)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), PdCl 2 (0.1 M aqueous solution 0.1 ml, 0.01 mmol) and ethyl lactate (27.8 mg, 0.24 mmol) were added to a 100 ml two-necked flat-bottomed flask and mixed into a mixed solution. .

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於150℃加熱12分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個 鈀奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 150 ° C for 12 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The aforementioned reduction reaction produces a plurality of Palladium nanoparticle, almost 0% by volume of the residue of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(33.6毫克，0.17毫莫耳)的水溶液50毫升作為介質，將前述的鈀奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱30分鐘，得到一鈀奈米粒子膠體溶液。 Finally, in step (c), the aforementioned palladium nanoparticle was dispersed in the two-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (33.6 mg, 0.17 mmol) as a medium, and the solution was Heating at 70 ° C for 30 minutes gave a palladium nanoparticle colloidal solution.

實施例63 使用γ-丁內酯作為還原劑以合成鈀奈米粒子膠體溶液 Example 63 Using γ-butyrolactone as a reducing agent to synthesize a palladium nanoparticle colloidal solution

首先，在步驟(a)中，將PdCl2(0.1M水溶液0.1毫升，0.01毫莫耳)和γ-丁內酯(20.3毫克，0.24毫莫耳)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), PdCl 2 (0.1 M aqueous solution 0.1 ml, 0.01 mmol) and γ-butyrolactone (20.3 mg, 0.24 mmol) were added to a 100 ml two-necked flat-bottomed flask and mixed into one. mixture.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於150℃加熱12分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個鈀奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 150 ° C for 12 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The above reduction reaction produces a residue containing a plurality of palladium nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(33.6毫克，0.17毫莫耳)的水溶液50毫升作為介質，將前述的鈀奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱30分鐘，得到一鈀奈米粒子膠體溶液。 Finally, in step (c), the aforementioned palladium nanoparticle was dispersed in the two-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (33.6 mg, 0.17 mmol) as a medium, and the solution was Heating at 70 ° C for 30 minutes gave a palladium nanoparticle colloidal solution.

實施例64 使用乳酸甲酯和檸檬酸作為組合還原劑以合成鈀奈米粒子膠體溶液 Example 64 Using methyl lactate and citric acid as a combined reducing agent to synthesize a palladium nanoparticle colloidal solution

首先，在步驟(a)中，將PdCl2(0.1M水溶液0.1毫升，0.01毫莫耳)和檸檬酸(45.7毫克，0.24毫莫耳)及乳酸甲酯(11.7毫克，0.11毫莫耳)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), PdCl 2 (0.1 M aqueous solution 0.1 ml, 0.01 mmol) and citric acid (45.7 mg, 0.24 mmol) and methyl lactate (11.7 mg, 0.11 mmol) were added. A 100 ml two-necked flat-bottomed flask was mixed and mixed into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於150℃加熱12分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個 鈀奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 150 ° C for 12 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The aforementioned reduction reaction produces a plurality of Palladium nanoparticle, almost 0% by volume of the residue of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(33.6毫克，0.17毫莫耳)的水溶液50毫升作為介質，將前述的鈀奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱30分鐘，得到一鈀奈米粒子膠體溶液。 Finally, in step (c), the aforementioned palladium nanoparticle was dispersed in the two-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (33.6 mg, 0.17 mmol) as a medium, and the solution was Heating at 70 ° C for 30 minutes gave a palladium nanoparticle colloidal solution.

實施例65 使用乳酸乙酯和檸檬酸作為組合還原劑以合成鈀奈米粒子膠體溶液 Example 65 Using ethyl lactate and citric acid as a combined reducing agent to synthesize a palladium nanoparticle colloidal solution

首先，在步驟(a)中，將PdCl2(0.1M水溶液0.1毫升，0.01毫莫耳)和檸檬酸(45.4毫克，0.24毫莫耳)及乳酸乙酯(11.9毫克，0.10毫莫耳)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), PdCl 2 (0.1 M aqueous solution 0.1 ml, 0.01 mmol) and citric acid (45.4 mg, 0.24 mmol) and ethyl lactate (11.9 mg, 0.10 mmol) were added. A 100 ml two-necked flat-bottomed flask was mixed and mixed into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於150℃加熱12分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個鈀奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 150 ° C for 12 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The above reduction reaction produces a residue containing a plurality of palladium nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(33.6毫克，0.17毫莫耳)的水溶液50毫升作為介質，將前述的鈀奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱30分鐘，得到一鈀奈米粒子膠體溶液。此外，如圖30的TEM影像所示，該鈀奈米粒子之平均粒徑為9nm至10nm。 Finally, in step (c), the aforementioned palladium nanoparticle was dispersed in the two-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (33.6 mg, 0.17 mmol) as a medium, and the solution was Heating at 70 ° C for 30 minutes gave a palladium nanoparticle colloidal solution. Further, as shown in the TEM image of FIG. 30, the palladium nanoparticle has an average particle diameter of 9 nm to 10 nm.

實施例66 使用乳酸和檸檬酸作為組合還原劑以合成鈀奈米粒子膠體溶液 Example 66 Using lactic acid and citric acid as a combined reducing agent to synthesize a palladium nanoparticle colloidal solution

首先，在步驟(a)中，將PdCl2(0.1M水溶液0.1毫升，0.01毫莫耳)和檸檬酸(45.7毫克，0.24毫莫耳)及乳酸(10.8毫克，0.12毫莫耳)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), PdCl 2 (0.1 M aqueous solution 0.1 ml, 0.01 mmol) and citric acid (45.7 mg, 0.24 mmol) and lactic acid (10.8 mg, 0.12 mmol) were added to 100 ml. The two-necked flat-bottomed flask was mixed and mixed into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於150℃加熱12分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個鈀奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 150 ° C for 12 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The above reduction reaction produces a residue containing a plurality of palladium nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(33.6毫克，0.17毫莫耳)的水溶液50毫升作為介質，將前述的鈀奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱30分鐘，得到一鈀奈米粒子膠體溶液。 Finally, in step (c), the aforementioned palladium nanoparticle was dispersed in the two-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (33.6 mg, 0.17 mmol) as a medium, and the solution was Heating at 70 ° C for 30 minutes gave a palladium nanoparticle colloidal solution.

實施例67 使用檸檬酸作為還原劑和分散劑以合成鈀奈米粒子膠體溶液 Example 67 Using citric acid as a reducing agent and dispersing agent to synthesize a palladium nanoparticle colloidal solution

首先，在步驟(a)中，將PdCl2(0.1M水溶液0.1毫升，0.01毫莫耳)和檸檬酸(45.2毫克，0.23毫莫耳)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in the step (a), PdCl 2 (0.1 M aqueous solution 0.1 ml, 0.01 mmol) and citric acid (45.2 mg, 0.23 mmol) were placed in a 100 ml two-necked flat-bottomed flask and mixed to form a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於150℃加熱12分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個鈀奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 150 ° C for 12 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The above reduction reaction produces a residue containing a plurality of palladium nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(33.6毫克，0.17毫莫耳)的水溶液50毫升作為介質，將前述的鈀奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱30分鐘，得到一鈀奈米粒子膠體溶液。 Finally, in step (c), the aforementioned palladium nanoparticle was dispersed in the two-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (33.6 mg, 0.17 mmol) as a medium, and the solution was Heating at 70 ° C for 30 minutes gave a palladium nanoparticle colloidal solution.

實施例68 使用聚乳酸作為還原劑以合成鋅奈米粒子膠體溶液 Example 68 Using polylactic acid as a reducing agent to synthesize a zinc nanoparticle colloidal solution

首先，在步驟(a)中，將ZnCl2(2M水溶液0.1毫升，0.2毫莫耳)和聚乳酸(106.5毫克)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in the step (a), ZnCl 2 (2 ml of an aqueous solution of 0.1 M, 0.2 mmol) and polylactic acid (106.5 mg) were placed in a 100 ml two-necked flat-bottomed flask and mixed to form a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於150℃加熱12分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個鋅奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 150 ° C for 12 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The above reduction reaction produces a residue containing a plurality of zinc nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(33.6毫克，0.17毫莫耳)的水溶液50毫升作為介質，將前述的鋅奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱30分鐘，得到一鋅奈米粒子膠體溶液。 Finally, in step (c), the aforementioned zinc nanoparticles were dispersed in the two-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (33.6 mg, 0.17 mmol) as a medium, and the solution was Heating at 70 ° C for 30 minutes gave a zinc nanoparticle colloidal solution.

實施例69 使用乳酸甲酯和檸檬酸作為組合還原劑以合成鋅奈米粒子膠體溶液 Example 69 Using methyl lactate and citric acid as a combined reducing agent to synthesize a zinc nanoparticle colloidal solution

首先，在步驟(a)中，將ZnCl2(2M水溶液0.1毫升，0.2毫莫耳)和檸檬酸(45.9毫克，0.24毫莫耳)及乳酸甲酯(10.4毫克，0.10毫莫耳)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), ZnCl 2 (2M aqueous solution 0.1 ml, 0.2 mmol) and citric acid (45.9 mg, 0.24 mmol) and methyl lactate (10.4 mg, 0.10 mmol) were added to 100. A two-neck flat-bottomed flask of cc was mixed and mixed into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於150℃加熱12分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個鋅奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 150 ° C for 12 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The above reduction reaction produces a residue containing a plurality of zinc nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(33.6毫克，0.17毫莫耳)的水溶液50毫升作為介質，將前述的鋅奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱30分鐘，得到一鋅奈米粒子膠體溶液。 Finally, in step (c), the aforementioned zinc nanoparticles were dispersed in the two-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (33.6 mg, 0.17 mmol) as a medium, and the solution was Heating at 70 ° C for 30 minutes gave a zinc nanoparticle colloidal solution.

實施例70 使用乳酸乙酯和檸檬酸作為組合還原劑以合成鋅奈米粒子膠體溶液 Example 70 Using ethyl lactate and citric acid as a combined reducing agent to synthesize a zinc nanoparticle colloidal solution

首先，在步驟(a)中，將ZnCl2(2M水溶液0.1毫升，0.2毫莫耳)和檸檬酸(45.9毫克，0.24毫莫耳)及乳酸乙酯(11.4毫克，0.10毫莫耳)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), ZnCl 2 (2M aqueous solution 0.1 ml, 0.2 mmol) and citric acid (45.9 mg, 0.24 mmol) and ethyl lactate (11.4 mg, 0.10 mmol) were added to 100. A two-neck flat-bottomed flask of cc was mixed and mixed into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於150℃加熱12分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個鋅奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 150 ° C for 12 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The above reduction reaction produces a residue containing a plurality of zinc nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(33.6毫克，0.17毫莫耳)的水溶液50毫升作為介質，將前述的鋅奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱30分鐘，得到一鋅奈米粒子膠體溶液。 Finally, in step (c), the aforementioned zinc nanoparticles were dispersed in the two-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (33.6 mg, 0.17 mmol) as a medium, and the solution was Heating at 70 ° C for 30 minutes gave a zinc nanoparticle colloidal solution.

實施例71 使用乳酸和檸檬酸作為組合還原劑以合成鋅奈米粒子膠體溶液 Example 71 Using lactic acid and citric acid as a combined reducing agent to synthesize a zinc nanoparticle colloidal solution

首先，在步驟(a)中，將ZnCl2(2M水溶液0.1毫升，0.2毫莫耳)和檸檬酸(45.9毫克，0.24毫莫耳)及乳酸(10.2毫克，0.11毫莫耳)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in step (a), ZnCl 2 (2M aqueous solution 0.1 ml, 0.2 mmol) and citric acid (45.9 mg, 0.24 mmol) and lactic acid (10.2 mg, 0.11 mmol) were added to 100 ml. A two-necked flat-bottomed flask was mixed and mixed into a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於150℃加熱12分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個鋅奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 150 ° C for 12 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The above reduction reaction produces a residue containing a plurality of zinc nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(33.6毫克，0.17毫莫耳)的水溶液50毫升作為介質，將前述的鋅奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱30分鐘，得到一鋅奈米粒子膠體溶液。此外，如圖31的TEM影像所示，該鋅奈米粒子之平均粒徑為26nm至27nm。 Finally, in step (c), the aforementioned zinc nanoparticles were dispersed in the two-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (33.6 mg, 0.17 mmol) as a medium, and the solution was Heating at 70 ° C for 30 minutes gave a zinc nanoparticle colloidal solution. Further, as shown in the TEM image of FIG. 31, the zinc nanoparticles have an average particle diameter of 26 nm to 27 nm.

實施例72 使用檸檬酸作為還原劑和分散劑以合成鋅奈米粒子膠體溶液 Example 72 Using Citric Acid as a Reducing Agent and Dispersing Agent to Synthesize a Zinc Nanoparticle Colloidal Solution

首先，在步驟(a)中，將ZnCl2(2M水溶液0.1毫升，0.2毫莫耳)和檸檬酸(45.9毫克，0.24毫莫耳)加入100毫升的雙頸平底燒瓶並混合成一混合溶液。 First, in the step (a), ZnCl 2 (2 ml aqueous solution of 0.1 ml, 0.2 mmol) and citric acid (45.9 mg, 0.24 mmol) were placed in a 100 ml two-necked flat-bottomed flask and mixed to form a mixed solution.

隨後，在步驟(b)中，將該雙頸平底燒瓶置於加熱板上於150℃加熱12分鐘以進行還原反應，且以IR光譜儀監測反應進行。前述還原反應產生含有複數個鋅奈米粒子、幾乎為前述混合溶液0體積%的殘餘物以及氯化氫氣體。在進行前述還原反應的同時，將還原反應中所產生的氯化氫氣體從連接至該雙頸平底燒瓶的回收口導至裝有10毫升水的錐形瓶進行收集。 Subsequently, in the step (b), the two-necked flat-bottomed flask was placed on a hot plate and heated at 150 ° C for 12 minutes to carry out a reduction reaction, and the reaction was monitored by an IR spectrometer. The above reduction reaction produces a residue containing a plurality of zinc nanoparticles, almost 0% by volume of the aforementioned mixed solution, and hydrogen chloride gas. While carrying out the aforementioned reduction reaction, hydrogen chloride gas generated in the reduction reaction was conducted from a recovery port connected to the two-necked flat-bottomed flask to an Erlenmeyer flask containing 10 ml of water for collection.

最後，在步驟(c)中，使用含有檸檬酸(33.6毫克，0.17毫莫耳)的水溶液50毫升作為介質，將前述的鋅奈米粒子分散於該雙頸平底燒瓶中，並將所述溶液以70℃加熱30分鐘，得到一鋅奈米粒子膠體溶液。 Finally, in step (c), the aforementioned zinc nanoparticles were dispersed in the two-necked flat-bottomed flask using 50 ml of an aqueous solution containing citric acid (33.6 mg, 0.17 mmol) as a medium, and the solution was Heating at 70 ° C for 30 minutes gave a zinc nanoparticle colloidal solution.

實驗結果討論 Discussion of experimental results

從實施例1至實施例56的結果，本創作採用四氯金酸水溶液作為金屬源，並且改變不同種類的還原劑以形成金奈米粒子，然後使用不同種類的介質來分散前述的金奈米粒子以獲得金奈米粒子膠體溶液。 From the results of Example 1 to Example 56, the present creation uses a tetrachloroauric acid aqueous solution as a metal source, and changes different kinds of reducing agents to form gold nanoparticles, and then uses different kinds of media to disperse the aforementioned gold nanoparticles. The particles are obtained to obtain a colloidal solution of the gold nanoparticles.

從實施例57至實施例61的結果，本創作採用硝酸銀水溶液作為金屬源，並且改變不同種類的還原劑以形成銀奈米粒子，然後使用不同種類的介質來分散前述的銀奈米粒子以獲得銀奈米粒子膠體溶液。 From the results of Example 57 to Example 61, the present invention employed an aqueous solution of silver nitrate as a metal source, and changed different kinds of reducing agents to form silver nanoparticles, and then used different kinds of media to disperse the aforementioned silver nanoparticles to obtain Silver nanoparticle colloidal solution.

從實施例62至實施例67的結果，本創作採用氯化鈀水溶液作為金屬源，並且改變不同種類的還原劑以形成鈀奈米粒子，然後使用不同種類的介質來分散前述的鈀奈米粒子以獲得鈀奈米粒子膠體溶液。 From the results of Example 62 to Example 67, the present work uses an aqueous solution of palladium chloride as a metal source, and changes different kinds of reducing agents to form palladium nanoparticles, and then uses different kinds of media to disperse the aforementioned palladium nanoparticles. A palladium nanoparticle colloidal solution is obtained.

從實施例68至實施例72的結果，本創作採用氯化鋅水溶液作為金屬源，並且改變不同種類的還原劑以形成鋅奈米粒子，然後使用不同種類的介質來分散前述的鋅奈米粒子以獲得鋅奈米粒子膠體溶液。 From the results of Example 68 to Example 72, the present invention uses an aqueous solution of zinc chloride as a metal source, and changes different kinds of reducing agents to form zinc nanoparticles, and then uses different kinds of media to disperse the aforementioned zinc nanoparticles. A zinc nanoparticle colloidal solution is obtained.

此外，實施例1至實施例34、實施例57至實施例59、實施例62至實施例65、以及實施例68至實施例70使用無毒且具有生物相容性的酯類作為還原劑，該酯類包括乳酸甲酯、乳酸乙酯、γ-丁內酯或聚乳酸等。因此，本創作對環境更友善且適合應用於現今社會。 Further, Examples 1 to 34, Examples 57 to 59, Examples 62 to 65, and Examples 68 to 70 use a non-toxic and biocompatible ester as a reducing agent. The esters include methyl lactate, ethyl lactate, γ-butyrolactone or polylactic acid. Therefore, this creation is more environmentally friendly and suitable for use in today's society.

從實施例1與實施例2的比較結果可知，由不同的λmax可以確定當選擇不同的分散介質分散金屬奈米粒子能製備出不同尺寸的金屬奈米粒子膠體溶液。同樣地，從實施例14與實施例15的比較結果也表示兩者具有不同的平均粒徑之金屬奈米粒子膠體溶液。此外，從實施例2、實施例15及實施例35的比較結果可知，由不同的λmax可以確定當選擇不同的還原劑能形成不同尺寸的金屬奈米粒子。由此可見，因本創作之製備方法是分成兩步驟進行而不是一鍋反應法(one pot reaction)，使得本創作具有更廣泛的選擇而可挑選出符合需求的還原劑與分散劑，進而能更方便地應用於各種工業或醫療應用。 From the comparison results of Example 1 and Example 2, it can be confirmed from different λ max that when different dispersing medium-dispersed metal nanoparticles are selected, colloidal solutions of metal nanoparticles of different sizes can be prepared. Similarly, the comparison results from Example 14 and Example 15 also indicate that the metal nanoparticle colloidal solution having different average particle diameters was used. Further, from the comparison results of Example 2, Example 15 and Example 35, it is understood that different λ max can be determined when different reducing agents can be selected to form metal nanoparticles of different sizes. It can be seen that since the preparation method of the present invention is carried out in two steps instead of one pot reaction, the creation has a wider selection and can select a reducing agent and a dispersing agent according to requirements, thereby enabling More convenient for a variety of industrial or medical applications.

與習知製備方法相比，實施例1至實施例72因進行還原反應時使用的水含量少而顯得金屬離子濃度相對較高，而讓製備金屬奈米粒子的反應時間可以縮短至80分鐘內，大部份的實施例的反應時間皆在20分鐘內，甚至最快只需2分鐘。由此可見，本創作確實是具有成本效益的方法，且因具有更快的還原速率，能使還原反應所得的金屬奈米粒子具有更窄的尺寸分佈結果。據 此，因該金屬奈米粒子具有均勻的尺寸大小而不需要進一步過濾，如此亦可使產率提高。 Compared with the conventional preparation method, the water content of Examples 1 to 72 used in the reduction reaction is relatively low, and the metal ion concentration is relatively high, and the reaction time for preparing the metal nanoparticles can be shortened to 80 minutes. In most of the examples, the reaction time is within 20 minutes, and even as fast as 2 minutes. Thus, this creation is indeed a cost-effective method, and because of the faster reduction rate, the metal nanoparticle obtained by the reduction reaction can have a narrower size distribution result. according to Thus, since the metal nanoparticles have a uniform size without further filtration, the yield can be improved.

不像習知的製備方法須包含將金屬離子溶液迅速加入沸騰之還原劑溶液的危險步驟，本創作的製備方法係加熱已預先混合的金屬離子溶液及還原劑，即使應用於大規模的製備需求也是非常安全的方法。此外，本創作藉由使用簡單的設置而不需使用複雜的反應設備或攪拌裝置，因此本創作能以簡單又有效率的方式進行。 Unlike conventional methods of preparation, which involve the dangerous step of rapidly adding a metal ion solution to a boiling reducing agent solution, the present preparation is a method of heating a pre-mixed metal ion solution and a reducing agent, even for large-scale preparation needs. It is also a very safe method. In addition, the creation can be performed in a simple and efficient manner by using simple setup without the use of complicated reaction equipment or agitating devices.

更重要的是，本創作使用有機還原劑及分散劑於水中，使得金屬奈米粒子膠體溶液可具有良好的品質與穩定性而可不售其他無機陽離子的干擾。 More importantly, the present invention uses organic reducing agents and dispersing agents in water, so that the metal nanoparticle colloidal solution can have good quality and stability without the interference of other inorganic cations.

此外，於本創作的步驟(b)中，加熱並將所產生的氣體導出該反應容器而可將陰離子(例如氯離子和硝酸根離子)轉化成氣體(例如氯化氫和二氧化氮)再被水捕捉而可回收再利用。由於大多數的陰離子從金屬奈米粒子膠體溶液中移除，使前述的金屬奈米粒子膠體溶液具有高穩定度及未受陰離子明顯干擾的界達電位值。 Furthermore, in step (b) of the present creation, heating and directing the generated gas out of the reaction vessel converts anions (such as chloride ions and nitrate ions) into gases (such as hydrogen chloride and nitrogen dioxide) and then water. Capture and recycle. Since most of the anions are removed from the colloidal solution of the metal nanoparticle, the aforementioned metal nanoparticle colloidal solution has a high stability and an exponential potential value that is not significantly disturbed by the anion.

儘管前述說明已闡述本創作的諸多特徵、優點及本創作的構成與特徵細節，然而這僅屬於示例性的說明。全部在本創作之申請專利範圍的一般涵義所表示範圍內，依據本創作原則所作的細節變化尤其是指形狀、尺寸和元件設置的改變，均仍屬於本創作的範圍內。 Although the foregoing description has set forth a number of features, advantages, and details of the composition and features of the present invention, this is merely exemplary. All of the changes in the general meaning of the scope of the patent application of this creation, the changes in detail according to this creative principle, especially the changes in shape, size and component settings, are still within the scope of this creation.

Claims (17)

一種製備金屬奈米粒子膠體溶液的方法，其包含以下步驟：步驟(a)：將一金屬水溶液和一還原劑於一反應容器中混合以形成一混合溶液；步驟(b)：加熱該混合溶液以進行還原反應而產生含有複數個金屬奈米粒子、反應殘餘物及氣體的一組合物；其中，該反應殘餘物的體積小於該混合溶液總體積的20%，並且將該氣體導出該反應容器；以及步驟(c)：用一介質分散該複數個金屬奈米粒子以獲得一金屬奈米粒子膠體溶液；其中，該金屬水溶液含有莫耳體積濃度為0.1M至3.0M的金屬離子，該金屬離子包括金離子、銀離子、銅離子、鋅離子、鎳離子、鈀離子、鈷離子、鐵離子、鈦離子、鎘離子、鉑離子、鋁離子、鉛離子、錳離子、鉻離子、鉬離子、釩離子或鎢離子；該還原劑包含一第一試劑或一聚酯，該第一試劑係選自一羧酸酯、一環酯、一檸檬酸、一乳酸、一乙醇酸、一抗壞血酸、一草酸、一酒石酸、一1,4-丁二醇、一甘油、一氫醌、一乙醛、一葡萄糖、一殼多醣及其組合；當該還原劑包含該第一試劑時，該第一試劑相對於該金屬離子的莫耳比為1至40；當該還原劑包含該聚酯時，該聚酯的重量為30毫克至150毫克。 A method for preparing a colloidal solution of a metal nanoparticle, comprising the steps of: (a): mixing an aqueous metal solution and a reducing agent in a reaction vessel to form a mixed solution; and step (b): heating the mixed solution Performing a reduction reaction to produce a composition comprising a plurality of metal nanoparticles, a reaction residue, and a gas; wherein the volume of the reaction residue is less than 20% of the total volume of the mixed solution, and the gas is led to the reaction vessel And step (c): dispersing the plurality of metal nanoparticles with a medium to obtain a metal nanoparticle colloidal solution; wherein the metal aqueous solution contains a metal ion having a molar volume concentration of 0.1 M to 3.0 M, the metal Ions include gold, silver, copper, zinc, nickel, palladium, cobalt, iron, titanium, cadmium, platinum, aluminum, lead, manganese, chromium, molybdenum, a vanadium ion or a tungsten ion; the reducing agent comprises a first reagent or a polyester, the first reagent is selected from the group consisting of a monocarboxylic acid ester, a monocyclic ester, a citric acid, a lactic acid, and a Alkyd, monoascorbic acid, monooxalic acid, monotartaric acid, monobutane 1,4-butanediol, monoglycerol, monohydroquinone, monoacetaldehyde, monoglucose, chitin and combinations thereof; when the reducing agent comprises the first In the case of a reagent, the molar ratio of the first reagent to the metal ion is from 1 to 40; when the reducing agent comprises the polyester, the polyester has a weight of from 30 mg to 150 mg. 如請求項1所述之方法，其中，該金屬水溶液還含有陰離子，該陰離子包括鹵離子或硝酸根離子。 The method of claim 1, wherein the aqueous metal solution further contains an anion comprising a halide ion or a nitrate ion. 如請求項2所述之方法，其中，該金屬離子來自於四氯金酸、硝酸銀、硝酸銅、二氯化銅、二氯化鋅、二氯化鎳、氯化鈀、二氯化鈷、二氯化鐵、三氯化鐵、二氯化鈦或四氯化鈦。 The method of claim 2, wherein the metal ion is derived from tetrachloroauric acid, silver nitrate, copper nitrate, copper dichloride, zinc dichloride, nickel dichloride, palladium chloride, cobalt dichloride, Ferric chloride, ferric chloride, titanium dichloride or titanium tetrachloride. 如請求項1所述之方法，其中，該步驟(b)中將該從還原反應生成的氣體導出該反應容器並包括使用一裝水的容器捕捉該氣體。 The method of claim 1, wherein the gas generated from the reduction reaction is taken out of the reaction vessel in the step (b) and comprises capturing the gas using a water-filled vessel. 如請求項1所述之方法，其中，該步驟(b)中的加熱溫度為50℃至150℃。 The method of claim 1, wherein the heating temperature in the step (b) is from 50 ° C to 150 ° C. 如請求項1所述之方法，其中，該步驟(b)中的加熱溫度為70℃至130℃。 The method of claim 1, wherein the heating temperature in the step (b) is from 70 ° C to 130 ° C. 如請求項1所述之方法，其中，該步驟(c)中的分散溫度為20℃至100℃。 The method of claim 1, wherein the dispersion temperature in the step (c) is from 20 ° C to 100 ° C. 如請求項1所述之方法，其中，該步驟(c)中的分散溫度為50℃至80℃。 The method of claim 1, wherein the dispersion temperature in the step (c) is from 50 ° C to 80 ° C. 如請求項1所述之方法，其中，該還原劑係該羧酸酯、該環酯、該聚酯或其組合。 The method of claim 1, wherein the reducing agent is the carboxylic acid ester, the cyclic ester, the polyester, or a combination thereof. 如請求項1所述之方法，其中，該羧酸酯為通式(I)所表示的 ；其中，通式(I)中的R為氫或甲基，而x為1至16的整數。 The method of claim 1, wherein the carboxylic acid ester is represented by the formula (I) Wherein R in the formula (I) is hydrogen or a methyl group, and x is an integer of from 1 to 16. 如請求項1所述之方法，其中，該環酯為通式(II)所表示的 ；其中，通式(II)中的環包含一氧原子及4至6個碳原子，而G為 氫、甲基或乙基。 The method of claim 1, wherein the cyclic ester is represented by the formula (II) Wherein the ring of the formula (II) contains an oxygen atom and 4 to 6 carbon atoms, and G is hydrogen, methyl or ethyl. 如請求項1所述之方法，其中，該聚酯為通式(III)所表示的 ；其中，通式(III)中的R為氫或甲基，及n為2至1400的整 數。 The method of claim 1, wherein the polyester is represented by the formula (III) Wherein R in the formula (III) is hydrogen or a methyl group, and n is an integer of from 2 to 1400. 如請求項1所述之方法，其中，該還原劑更包括一聚乙二醇、一纖維素、一羧甲基纖維素、一環糊精、一殼聚醣或其組合。 The method of claim 1, wherein the reducing agent further comprises a polyethylene glycol, a cellulose, a carboxymethyl cellulose, a cyclodextrin, a chitosan or a combination thereof. 如請求項1所述之方法，其中，該步驟(c)中的該介質包含一分散劑水溶液，而該分散劑水溶液包括一檸檬酸水溶液、一乳酸水溶液、一聚乳酸水溶液、一氫氧化鈉水溶液、一十六烷基胺水溶液、一油胺水溶液、一四辛基溴化銨水溶液、一十二烷硫醇水溶液、一聚環氧乙烷水溶液、一聚乙烯吡咯烷酮水溶液或其組合。 The method of claim 1, wherein the medium in the step (c) comprises an aqueous solution of a dispersant, and the aqueous solution of the dispersant comprises an aqueous solution of citric acid, an aqueous solution of lactic acid, an aqueous solution of polylactic acid, and a sodium hydroxide. An aqueous solution, an aqueous solution of hexadecylamine, an aqueous solution of oleylamine, an aqueous solution of tetraoctyl ammonium bromide, an aqueous solution of dodecanethiol, an aqueous solution of polyethylene oxide, an aqueous solution of polyvinylpyrrolidone or a combination thereof. 如請求項14所述之方法，其中，該分散劑的莫耳體積濃度為0.001M至0.1M。 The method of claim 14, wherein the dispersant has a molar volume concentration of from 0.001 M to 0.1 M. 如請求項14所述之方法，其中，該分散劑相對於該等金屬奈米粒子的莫耳比為10至100。 The method of claim 14, wherein the dispersant has a molar ratio of from 10 to 100 with respect to the metal nanoparticles. 如請求項14所述之方法，其中，該分散劑相對於該等金屬奈米粒子的莫耳比為15至30。 The method of claim 14, wherein the dispersing agent has a molar ratio of 15 to 30 with respect to the metal nanoparticles.
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